CN106698364A - Production method for thionyl chloride - Google Patents
Production method for thionyl chloride Download PDFInfo
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- CN106698364A CN106698364A CN201710051340.0A CN201710051340A CN106698364A CN 106698364 A CN106698364 A CN 106698364A CN 201710051340 A CN201710051340 A CN 201710051340A CN 106698364 A CN106698364 A CN 106698364A
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- Prior art keywords
- thionyl chloride
- gas
- liquid phase
- reactor
- rectifying column
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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
- C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
- C01B17/4561—Compounds containing sulfur, halogen and oxygen only
- C01B17/4584—Thionyl chloride (SOCl2)
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the technical field of chemical production, and particularly relates to a production method for thionyl chloride. The production method comprises the following step: introducing synthesis gas generated by reaction, in a reaction kettle, of sulfur and chlorine gas, and sulfur dioxide gas into a reactor, and enabling a crude product thionyl chloride generated by the reactor to directly enter a splitter in the form of gas after passing through an absorption tower; introducing gas-phase crude product thionyl chloride from the splitter to enter a rectifying column, condensing gas-phase on the top of the rectifying tower, and introducing the condensed gas-phase into a reflux tank; introducing the gas phase in the reflux tank to enter a vacuum-pumping tank through an ejector and alloying a synthesis kettle in a circulating mode, and recovering a qualified product from the middle part of the rectifying column. According to the production method, a light component in the crude product thionyl chloride is converted into a heavy component through the adsorption tower, and pressure drop before and after conversion is relatively small, operation is easy, automation is easily realized and conversion is more complete by adopting the tower, so that the load of the rectifying system is greatly reduced.
Description
Technical field
The invention belongs to chemical production technical field, and in particular to a kind of production method of thionyl chloride.
Background technology
ZL95110380.6 discloses a kind of manufacture method of thionyl chloride, and the method is will to catalyze and synthesize obtained chlorination
Sulfoxide through cool down liquid thionyl chloride crude product is squeezed into and is previously added in the distillation still of Cosan, obtain liquid by batch fractionating
Sulphoxide chloride product.
According to document introduction in the preparation process of thionyl chloride, by the thionyl chloride crude product of reactor synthesis through supercooling
Batch fractionating is carried out again after solidifying or carries out the rectifying of two stage rectification tower/three-level rectifying column.
Reactor gas phase crude product thionyl chloride out is condensed in thionyl chloride preparation process, carry out essence with liquid phase after sulphur
Evaporate, and gas phase then recycled return reaction system；The condensed rear enclosure of tail gas for being produced in distillation process simultaneously uses back reaction system,
But all of tail gas can not all be condensed, cause certain loss of material, the tail gas not cooled down is needed by water
Absorb, Alkali absorption is emptied after processing, technique is relative complex and causes material loss；The use of excessive condenser simultaneously pacifies device
Full performance is substantially reduced；Regasified after crude product thionyl chloride is condensed and cause certain steam consumption, and need to be equipped with accordingly
Power-equipment, energy consumption is higher；Reactor gas phase crude product thionyl chloride out increases rectifying column if rectifying column is directly entered
Produce load；Chlorosulfuric acid containing 0.3%-0.5% in thionyl chloride finished product.
The content of the invention
It is an object of the invention to provide a kind of production method of thionyl chloride, improve product quality, improve product receipts
Rate, energy consumption is reduced, the disposal ability of rectifying column is improve and is improve the security of device.
The production method of thionyl chloride of the present invention, step is as follows：
(1) sulphur and chlorine react the synthesis gas of generation in synthesis reactor and enter reactor together with sulfur dioxide gas,
It is direct in the form of a vapor by entering decomposer, absorption tower behind absorption tower by the crude product thionyl chloride of reactor reaction generation
In liquid phase enter receiving tank；
(2) the gas phase crude product thionyl chloride by decomposer out enters rectifying column, and liquid phase circulation applies mechanically bout in receiving tank
Into kettle, the heavy constituent recycled that rectifying column bottom produces returns synthesis reactor, return tank is entered after rectifying tower top gas phase is condensed, flows back
Partial Liquid Phase is beaten to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied mechanically back in remaining liquid phase extraction in return tank；
(3) gas phase in return tank applies mechanically back synthesis reactor, the extraction of rectifying column middle part through injector into tank Posterior circle is evacuated
Qualified products.
Partial Liquid Phase and the volume ratio of remaining liquid phase described in step (2) are 4-10:1.
Whole system pressure of the present invention is between 0-1.0MPa.
Second pump provides power to tank is evacuated.
The continuous technique for preparing thionyl chloride of present invention optimization, makes whole thionyl chloride production realize on practical significance
It is closed, from truly realizing zero-emission.
The present invention compared with prior art, has the advantages that：
Thionyl chloride production of the present invention is totally-enclosed circulation production, and without waste water,waste gas and industrial residue discharge, product yield is basic
Reach 100%.This invention simplifies production technology, the condensation of the crude product thionyl chloride for reflecting is eliminated, with sulphur, light component
The technique such as apply mechanically；Because thionyl chloride is clear to water decomposition as hydrogen chloride, sulfur dioxide, The present invention reduces making for condenser
With so as to reduce the probability that thionyl chloride contacts water, reduce causes system overpressure, burn into leak because of condenser leak
Probability, substantially increase equipment safety；Simultaneously because reducing the process that condensation is regasified, the energy of device is greatly reduced
Consumption；The sulfonyl chlorinity in thionyl chloride finished product is set to be reduced to less than 0.1% due to reasonable employment decomposer；As a result of suction
Light component in crude product thionyl chloride is converted into heavy constituent by the mode for receiving tower, and pressure drop change is smaller before and after conversion, it is easy to grasp
Make, it is easy to automate and caused by the way of tower conversion it is more thorough, while greatly reducing the load of distillation system.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention；
In figure：1st, synthesis reactor；2nd, reactor；3rd, absorption tower；4th, decomposer；5th, rectifying column；6th, condenser；7th, return tank；
8th, injector；9th, tank is evacuated；10th, the first pump；11st, the second pump；12nd, receiving tank；13rd, the 3rd pump.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
(1) sulphur and chlorine react the synthesis gas of generation in synthesis reactor and enter reactor together with sulfur dioxide gas,
It is direct in the form of a vapor by entering decomposer, absorption tower behind absorption tower by the crude product thionyl chloride of reactor reaction generation
In liquid phase enter receiving tank；
(2) the gas phase crude product thionyl chloride by decomposer out enters rectifying column, and liquid phase circulation applies mechanically bout in receiving tank
Into kettle, the heavy constituent recycled that rectifying column bottom produces returns synthesis reactor, return tank is entered after rectifying tower top gas phase is condensed, flows back
Partial Liquid Phase is beaten to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied mechanically back in remaining liquid phase extraction in return tank；Part
Liquid phase is 8 with the volume ratio of remaining liquid phase:1；
(3) gas phase in return tank applies mechanically back synthesis reactor, the extraction of rectifying column middle part through injector into tank Posterior circle is evacuated
Qualified products.
Embodiment 2
(1) sulphur and chlorine react the synthesis gas of generation in synthesis reactor and enter reactor together with sulfur dioxide gas,
It is direct in the form of a vapor by entering decomposer, absorption tower behind absorption tower by the crude product thionyl chloride of reactor reaction generation
In liquid phase enter receiving tank；
(2) the gas phase crude product thionyl chloride by decomposer out enters rectifying column, and liquid phase circulation applies mechanically bout in receiving tank
Into kettle, the heavy constituent recycled that rectifying column bottom produces returns synthesis reactor, return tank is entered after rectifying tower top gas phase is condensed, flows back
Partial Liquid Phase is beaten to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied mechanically back in remaining liquid phase extraction in return tank；Part
Liquid phase is 10 with the volume ratio of remaining liquid phase:1；
(3) gas phase in return tank applies mechanically back synthesis reactor, the extraction of rectifying column middle part through injector into tank Posterior circle is evacuated
Qualified products.
Embodiment 3
(1) sulphur and chlorine react the synthesis gas of generation in synthesis reactor and enter reactor together with sulfur dioxide gas,
It is direct in the form of a vapor by entering decomposer, absorption tower behind absorption tower by the crude product thionyl chloride of reactor reaction generation
In liquid phase enter receiving tank；
(2) the gas phase crude product thionyl chloride by decomposer out enters rectifying column, and liquid phase circulation applies mechanically bout in receiving tank
Into kettle, the heavy constituent recycled that rectifying column bottom produces returns synthesis reactor, return tank is entered after rectifying tower top gas phase is condensed, flows back
Partial Liquid Phase is beaten to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied mechanically back in remaining liquid phase extraction in return tank；Part
Liquid phase is 4 with the volume ratio of remaining liquid phase:1；
(3) gas phase in return tank applies mechanically back synthesis reactor, the extraction of rectifying column middle part through injector into tank Posterior circle is evacuated
Qualified products.
Claims (2)
1. a kind of production method of thionyl chloride, it is characterised in that step is as follows：
(1) sulphur and chlorine react the synthesis gas of generation in synthesis reactor and enter reactor together with sulfur dioxide gas, pass through
The crude product thionyl chloride of reactor reaction generation is direct in the form of a vapor by entering decomposer behind absorption tower, in absorption tower
Liquid phase enters receiving tank；
(2) the gas phase crude product thionyl chloride by decomposer out enters rectifying column, and liquid phase circulation applies mechanically back synthesis reactor in receiving tank,
The heavy constituent recycled that rectifying column bottom produces returns synthesis reactor, return tank is entered after rectifying tower top gas phase is condensed, in return tank
Partial Liquid Phase is beaten to rectifying column through the first pump and returns stream, and synthesis reactor is applied mechanically back in remaining liquid phase extraction in return tank；
(3) gas phase in return tank applies mechanically back synthesis reactor through injector into tank Posterior circle is evacuated, and the extraction of rectifying column middle part is qualified
Product.
2. the production method of thionyl chloride according to claim 1, it is characterised in that the Partial Liquid Phase described in step (2)
It is 4-10 with the volume ratio of remaining liquid phase:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710051340.0A CN106698364B (en) | 2017-01-23 | 2017-01-23 | The production method of thionyl chloride |
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| CN201710051340.0A CN106698364B (en) | 2017-01-23 | 2017-01-23 | The production method of thionyl chloride |
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| CN106698364A true CN106698364A (en) | 2017-05-24 |
| CN106698364B CN106698364B (en) | 2019-03-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453704A (en) * | 2019-01-18 | 2020-07-28 | 江西世龙实业股份有限公司 | Device and method for recycling tail gas generated in thionyl chloride production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284652A (en) * | 2008-01-30 | 2008-10-15 | 江西电化精细化工有限责任公司 | Liquid phase circulation method in synthesis of thionyl chloride |
| CN103043620A (en) * | 2012-12-31 | 2013-04-17 | 山东凯盛新材料股份有限公司 | Method for recycling tail gas during thionyl chloride preparation |
| CN106315519A (en) * | 2016-08-29 | 2017-01-11 | 山东凯盛新材料股份有限公司 | Method for preparing thionyl chloride |
| CN106335881A (en) * | 2016-08-29 | 2017-01-18 | 山东凯盛新材料股份有限公司 | Technology for preparing thionyl chloride |
-
2017
- 2017-01-23 CN CN201710051340.0A patent/CN106698364B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284652A (en) * | 2008-01-30 | 2008-10-15 | 江西电化精细化工有限责任公司 | Liquid phase circulation method in synthesis of thionyl chloride |
| CN103043620A (en) * | 2012-12-31 | 2013-04-17 | 山东凯盛新材料股份有限公司 | Method for recycling tail gas during thionyl chloride preparation |
| CN106315519A (en) * | 2016-08-29 | 2017-01-11 | 山东凯盛新材料股份有限公司 | Method for preparing thionyl chloride |
| CN106335881A (en) * | 2016-08-29 | 2017-01-18 | 山东凯盛新材料股份有限公司 | Technology for preparing thionyl chloride |
Non-Patent Citations (4)
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| 丁伟 等: ""由硫磺、氯气一步法制备二氯化硫"", 《精细化工》 * |
| 吴祖杰 等: ""氯化亚砜连续精馏系统的改进"", 《盐业与化工》 * |
| 张丹: ""直接合成法一氯化硫生产技术探讨"", 《化工中间体》 * |
| 张瑞芹: ""二氯化硫的制备工艺"", 《河北化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453704A (en) * | 2019-01-18 | 2020-07-28 | 江西世龙实业股份有限公司 | Device and method for recycling tail gas generated in thionyl chloride production |
| CN111453704B (en) * | 2019-01-18 | 2021-11-23 | 江西世龙实业股份有限公司 | Device and method for recycling tail gas generated in thionyl chloride production |
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| CN106698364B (en) | 2019-03-15 |
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