CN106698364B - The production method of thionyl chloride - Google Patents
The production method of thionyl chloride Download PDFInfo
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- CN106698364B CN106698364B CN201710051340.0A CN201710051340A CN106698364B CN 106698364 B CN106698364 B CN 106698364B CN 201710051340 A CN201710051340 A CN 201710051340A CN 106698364 B CN106698364 B CN 106698364B
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- thionyl chloride
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- liquid phase
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- 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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to chemical production technical fields, and in particular to a kind of production method of thionyl chloride.The synthesis gas that sulphur and chlorine react generation in synthesis reactor enters reactor together with sulfur dioxide gas, directly enters decomposer behind absorption tower in the form of a vapor by the crude product thionyl chloride that reactor reaction generates；Rectifying column is entered by the gas phase crude product thionyl chloride that decomposer comes out, rectifying tower top gas phase enters return tank after condensing；Gas phase in return tank produces qualified products in recycled time synthesis reactor, rectifying column middle part after injector enters and evacuates tank.The present invention is due to converting heavy constituent for the light component in crude product thionyl chloride by the way of absorption tower, the pressure drop variation of conversion front and back is smaller, it is easily operated, easy to automate and make conversion more thorough by the way of tower, while greatly reducing the load of distillation system.
Description
Technical field
The invention belongs to chemical production technical fields, and in particular to a kind of production method of thionyl chloride.
Background technique
ZL95110380.6 discloses a kind of manufacturing method of thionyl chloride, and this method is will to catalyze and synthesize chlorination obtained
Sulfoxide obtains liquid by batch fractionating through cooling that liquid thionyl chloride crude product is squeezed into the distillation still for being previously added sulphur powder
Sulphoxide chloride product.
According to document introduction in the preparation process of thionyl chloride, the thionyl chloride crude product by reactor synthesis is through being subcooled
Batch fractionating is carried out after solidifying again or carries out the rectifying of two stage rectification tower/three-level rectifying column.
The gas phase crude product thionyl chloride that reactor comes out in thionyl chloride preparation process is condensed, carries out essence with liquid phase after sulphur
It evaporates, and then recycled returns reaction system to gas phase；The tail gas generated in distillation process simultaneously uses back reaction system through condensing rear enclosure,
But all tail gas can not all be condensed, certain loss of material is caused, the tail gas not cooled down is needed by water
It absorbs, emptied after Alkali absorption processing, technique is relative complex and causes material loss；The use of excessive condenser pacifies device simultaneously
Full performance substantially reduces；Crude product thionyl chloride regasifies after condensing causes certain steam consumption, and needs to be equipped with corresponding
Power-equipment, energy consumption are higher；The gas phase crude product thionyl chloride that reactor comes out increases rectifying column if being directly entered rectifying column
Produce load；Contain the chlorosulfuric acid of 0.3%-0.5% in thionyl chloride finished product.
Summary of the invention
The object of the present invention is to provide a kind of production methods of thionyl chloride, improve product quality, improve product receipts
Rate reduces energy consumption, improves the processing capacity of rectifying column and improve the safety of device.
The production method of thionyl chloride of the present invention, steps are as follows:
(1) synthesis gas that sulphur and chlorine react generation in synthesis reactor enters reactor together with sulfur dioxide gas,
Directly enter decomposer, absorption tower behind absorption tower in the form of a vapor by the crude product thionyl chloride that reactor reaction generates
In liquid phase enter receiving tank；
(2) rectifying column is entered by the gas phase crude product thionyl chloride that decomposer comes out, liquid phase circulation applies bout in receiving tank
At kettle, the heavy constituent recycled that rectifying column bottom generates returns synthesis reactor, and rectifying tower top gas phase enters return tank, reflux after condensing
Partial Liquid Phase beats to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied back in remaining liquid phase extraction in return tank；
(3) recycled after injector enters and evacuates tank of the gas phase in return tank returns synthesis reactor, extraction in the middle part of rectifying column
Qualified products.
The volume ratio of Partial Liquid Phase described in step (2) and remaining liquid phase is 4-10:1.
Whole system pressure of the present invention is between 0-1.0MPa.
Second pump provides power to tank is evacuated.
Present invention optimization continuously prepares the technique of thionyl chloride, realizes entire thionyl chloride production on practical significance
It is closed, from truly realizing zero-emission.
Compared with prior art, the present invention having the following beneficial effects:
Thionyl chloride production of the present invention is totally-enclosed circulation production, and no waste water,waste gas and industrial residue discharges, and product yield is basic
Reach 100%.This invention simplifies production technology, the condensation of the crude product thionyl chloride reflected is eliminated, with sulphur, light component
The techniques such as apply；Since thionyl chloride is clear to water decomposition as hydrogen chloride, sulfur dioxide, The present invention reduces making for condenser
With to reduce the probability of thionyl chloride contact water, reducing leads to system overpressure, burn into leakage because of condenser leak
Probability, substantially increase equipment safety；Simultaneously because reducing the process that condensation regasifies, the energy of device is greatly reduced
Consumption；Since reasonable employment decomposer makes the sulfonyl chlorinity in thionyl chloride finished product be reduced to 0.1% or less；It is inhaled due to using
The light component in crude product thionyl chloride is converted heavy constituent by the mode for receiving tower, and the pressure drop variation of conversion front and back is smaller, is easy to grasp
Make, is easy to automate and make to convert using tower by the way of more thorough, while greatly reducing the load of distillation system.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention；
In figure: 1, synthesis reactor；2, reactor；3, absorption tower；4, decomposer；5, rectifying column；6, condenser；7, return tank；
8, injector；9, tank is evacuated；10, the first pump；11, the second pump；12, receiving tank；13, third pump.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
(1) synthesis gas that sulphur and chlorine react generation in synthesis reactor enters reactor together with sulfur dioxide gas,
Directly enter decomposer, absorption tower behind absorption tower in the form of a vapor by the crude product thionyl chloride that reactor reaction generates
In liquid phase enter receiving tank；
(2) rectifying column is entered by the gas phase crude product thionyl chloride that decomposer comes out, liquid phase circulation applies bout in receiving tank
At kettle, the heavy constituent recycled that rectifying column bottom generates returns synthesis reactor, and rectifying tower top gas phase enters return tank, reflux after condensing
Partial Liquid Phase beats to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied back in remaining liquid phase extraction in return tank；Part
The volume ratio of liquid phase and remaining liquid phase is 8:1；
(3) recycled after injector enters and evacuates tank of the gas phase in return tank returns synthesis reactor, extraction in the middle part of rectifying column
Qualified products.
Embodiment 2
(1) synthesis gas that sulphur and chlorine react generation in synthesis reactor enters reactor together with sulfur dioxide gas,
Directly enter decomposer, absorption tower behind absorption tower in the form of a vapor by the crude product thionyl chloride that reactor reaction generates
In liquid phase enter receiving tank；
(2) rectifying column is entered by the gas phase crude product thionyl chloride that decomposer comes out, liquid phase circulation applies bout in receiving tank
At kettle, the heavy constituent recycled that rectifying column bottom generates returns synthesis reactor, and rectifying tower top gas phase enters return tank, reflux after condensing
Partial Liquid Phase beats to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied back in remaining liquid phase extraction in return tank；Part
The volume ratio of liquid phase and remaining liquid phase is 10:1；
(3) recycled after injector enters and evacuates tank of the gas phase in return tank returns synthesis reactor, extraction in the middle part of rectifying column
Qualified products.
Embodiment 3
(1) synthesis gas that sulphur and chlorine react generation in synthesis reactor enters reactor together with sulfur dioxide gas,
Directly enter decomposer, absorption tower behind absorption tower in the form of a vapor by the crude product thionyl chloride that reactor reaction generates
In liquid phase enter receiving tank；
(2) rectifying column is entered by the gas phase crude product thionyl chloride that decomposer comes out, liquid phase circulation applies bout in receiving tank
At kettle, the heavy constituent recycled that rectifying column bottom generates returns synthesis reactor, and rectifying tower top gas phase enters return tank, reflux after condensing
Partial Liquid Phase beats to rectifying column through the first pump and returns stream in tank, and synthesis reactor is applied back in remaining liquid phase extraction in return tank；Part
The volume ratio of liquid phase and remaining liquid phase is 4:1；
(3) recycled after injector enters and evacuates tank of the gas phase in return tank returns synthesis reactor, extraction in the middle part of rectifying column
Qualified products.
Claims (2)
1. a kind of production method of thionyl chloride, it is characterised in that steps are as follows:
(1) synthesis gas that sulphur and chlorine react generation in synthesis reactor enters reactor together with sulfur dioxide gas, passes through
The crude product thionyl chloride that reactor reaction generates directly enters decomposer behind absorption tower in the form of a vapor, in absorption tower
Liquid phase enters receiving tank；
(2) rectifying column being entered by the gas phase crude product thionyl chloride that decomposer comes out, liquid phase circulation applies back synthesis reactor in receiving tank,
The heavy constituent recycled that rectifying column bottom generates returns synthesis reactor, and rectifying tower top gas phase enters return tank after condensing, in return tank
Partial Liquid Phase beats to rectifying column through the first pump and returns stream, and synthesis reactor is applied back in remaining liquid phase extraction in return tank；
(3) recycled after injector enters and evacuates tank of the gas phase in return tank returns synthesis reactor, and extraction is qualified in the middle part of rectifying column
Product.
2. the production method of thionyl chloride according to claim 1, it is characterised in that Partial Liquid Phase described in step (2)
Volume ratio with remaining liquid phase is 4-10:1.
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| 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 CN106698364A (en) | 2017-05-24 |
| CN106698364B true CN106698364B (en) | 2019-03-15 |
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| 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 |
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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| "二氯化硫的制备工艺";张瑞芹;《河北化工》;20080430;第31卷(第4期);第43-44页 |
| "氯化亚砜连续精馏系统的改进";吴祖杰 等;《盐业与化工》;20130731;第42卷(第7期);第42-44页 |
| "由硫磺、氯气一步法制备二氯化硫";丁伟 等;《精细化工》;19991231;第16卷(第3期);第60-62页 |
| "直接合成法一氯化硫生产技术探讨";张丹;《化工中间体》;20081231(第09期);第54-57页 |
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