CN106829878B - Dichloride sulphur preparing process and preparation facilities - Google Patents
Dichloride sulphur preparing process and preparation facilities Download PDFInfo
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- CN106829878B CN106829878B CN201611182523.8A CN201611182523A CN106829878B CN 106829878 B CN106829878 B CN 106829878B CN 201611182523 A CN201611182523 A CN 201611182523A CN 106829878 B CN106829878 B CN 106829878B
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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
- C01B17/4507—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only
- C01B17/4538—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only containing sulfur and chlorine only
- C01B17/4546—Sulfur dichloride
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Abstract
The invention discloses a kind of dichloride sulphur preparing process and preparation facilities, the preparation method comprises the following steps: using sulfur monochloride and chlorine as raw material 60 DEG C~120 DEG C at a temperature of carry out synthetic reaction, resulting gaseous mixture enters the catalytic reactor for loading silica, catalysis reaction is carried out at 60 DEG C~90 DEG C, products therefrom is collected after condensing, and obtains liquid sulfur dichloride.Preparation facilities includes the reaction solution kettle being sequentially communicated, catalytic reactor, condenser and receives kettle, reaction solution kettle is equipped with snorkel, catalytic reactor includes catalytic reaction tube and the heating tube that is sheathed on outside it, catalytic reaction tube both ends open, one end is connect with reaction solution kettle, the other end is connect with condenser, and heating tube one end is equipped with heating medium inlet, and the other end is equipped with Crude product input.The preparation method has many advantages, such as simple process, remains without catalyst, without distillation, product purity and high income.The device is easy to operate, continuous-stable, and no waste generates.
Description
Technical field
The invention belongs to inorganic chemical product preparation technical field more particularly to a kind of dichloride sulphur preparing process and systems
Standby device.
Background technique
Sulfur dichloride is important inorganic chemical product, molecular structural formula SCl2, it is widely used in organic synthesis, manufactures
The oxide of acid anhydrides or organic acid, the additive of high pressure lubricant and cutting pool, is handled plant oil (such as corn oil, soybean oil)
Working process agent.Also act as disinfectant and fungicide.
CN95110380 discloses a kind of synthetic method of sulfur dichloride, is closed at 30~80 DEG C using sulphur and chlorine
At obtaining sulfur monochloride, then controls 30~80 DEG C of reaction temperature chlorine is passed through in sulfur monochloride liquid and sulfur dichloride gas is made
Body.This method reaction speed is slow, and yield is not reported.
CN91104832 discloses a kind of synthetic method of sulfur dichloride, is closed at 30~80 DEG C using sulphur and chlorine
At obtaining sulfur monochloride, then 30~80 DEG C of reaction temperature are controlled, in catalyst Fe Cl3(or Fe powder, FeCl2、A1Cl3) exist
Under the conditions of chlorine is passed through in sulfur monochloride liquid, sulfur dichloride is made, yield do not report.
CN1473758A discloses a kind of dichloride sulphur preparing process, using sulfur monochloride 0 under Louis acid catalysis
~10 DEG C are passed through chlorine and prepare sulfur dichloride, catalyst (the Fe powder, Fe of addition2S 、FeCl3、A1Cl3Deng) it is partly dissolved in two
It in sulfur chloride, is partially suspended in sulfur dichloride with molecule, remainder is deposited in reaction kettle bottom.Using sulfur dichloride
To have strict demand to the amount of wherein residual catalyst when other products of Material synthesis, in order to avoid influence the content of downstream product, receive
Rate and properties of product.Prior art is mostly to remove solid catalyst by the way of filtering, then remove sulfur dichloride through distilling
In the catalyst that dissolves.
CN104098072A discloses one kind to load ferric trichloride granular active carbon FeCl3/ C is catalyst, with a chlorine
Changing sulphur and chlorine is reaction raw materials and carrier gas, and the mixed gas of chlorine and sulfur monochloride after vaporization enters fixed-bed catalytic tubular type
Reactor, the technique that continuous gas-phase catalysis prepares sulfur dichloride.There are following three disadvantages for the technique: first is that needing a chlorine
Change sulphur to be gasified totally, it is more demanding to consersion unit；Second is that chlorine and sulfur monochloride molar ratio are 5: 10~1, one way chlorine disappears
Consumption is big；Third is that sulfur dichloride generated is liquid since catalytic reaction temperature is 30~50 DEG C, in catalyst it is effective at
Divide FeCl3It has and is dissolved in liquid sulfur dichloride on a small quantity, influence the purity of product.
US3219413 reports a kind of synthetic method of continuous production sulfur dichloride, using industrial sulphur 80~125
It is passed through chlorine under the conditions of DEG C, obtains Sulphur Monochloride and sulphur dichloride mixture, a certain amount of Fe powder is added in liquefied mixture
(or Fe2S、FeC13), 80~125 DEG C of conditions lead to the distillation of chlorine side below, and excessive chlorine is applied to sulfur monochloride synthesis.The method
Sulfur dichloride crude product is first obtained by synthesis, sulfur dichloride is then obtained by distillation, but this method uses catalyst, when distillation
Sulfur dichloride decomposes seriously, and products obtained therefrom purity is low, and plant capacity is low.
US3071441 discloses a kind of distillating method of sulfur dichloride, in the crude product that sulfur monochloride is synthesized with chlorine
Charged material weight, 0.2~1.0% PCl are added in sulfur dichloride5Stabilizer is distilled, and distillation yield is less than 65%.
US3071442 discloses a kind of distillating method of sulfur dichloride, in the crude product that sulfur monochloride is synthesized with chlorine
The stabilizers such as phosphite ester or phosphorous acid hydrogen ester are added in sulfur dichloride to distill through row, Asia is being added less than 70% in distillation yield
Exothermic reaction can occur when phosphate or hydrogen phosphite esters stabilizer, may cause stabilizer nature.Since sulfur dichloride exists
It decomposes reaction in distillation process vulnerable to heat, a certain amount of sulfur monochloride, remaining kettle liquid is still contained in the product distilled
For the mixture of a large amount of sulfur monochlorides and a small amount of sulfur dichloride.The mixture is in the case where containing phosphorus trioxide stabilizer, no
It can react again with chlorine for synthesizing sulfur dichloride.Therefore sulfur dichloride crude product can generate a large amount of useless in distillation process
Liquid and exhaust gas, pollute the environment.
Above-mentioned technique has the disadvantage in that mostly
1, since sulfur monochloride reacts to obtain sulfur dichloride to be reversible reaction, in the case where chlorine not excess, reaction is easy
It is carried out toward back reaction direction, therefore traditional handicraft is difficult to accomplish the sulfur dichloride of high conversion and high-content.
2, traditional handicraft can remove most of catalyst using filtering, but still have partial catalyst to be dissolved in sulfur dichloride production
In product, the quality of product is influenced, distillation is carried out and isolates catalyst.Reversible due to reacting, temperature increases when distillation, reaction
Reverse direction carries out, and decomposes sulfur dichloride and generates sulfur monochloride and chlorine, generates largely kettle liquid and chlorine containing sulfur monochloride
Tail gas causes damages to environment.
3, when distilling sulfur dichloride, a certain amount of phosphorus trichloride (or phosphorus pentachloride etc.) is added into distillate and stablizes
Agent can make distillation yield be increased to 83%.But it will be (or phosphoric containing a certain amount of phosphorus trichloride in the kettle liquid after distilling
Phosphorus etc.), under the conditions of having existing for stabilizer, distillation kettle liquid cannot be again with chlorine reaction, and causing distillation kettle liquid that cannot recycle makes
With, it can only be as liquid waste processing, quantity of three wastes is big.
4, the sulfur dichloride product content that traditional handicraft distills is less than 85%.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, a kind of simple process is provided, without catalyst
It remains, without distillation, product purity and high income, the sulfur dichloride preparation method generated without waste, in addition, also providing one kind
Preparation facilities used in the preparation method.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of dichloride sulphur preparing process, using sulfur monochloride and chlorine as raw material 60 DEG C~120 DEG C at a temperature of into
Row synthetic reaction, resulting gaseous mixture enter the catalytic reactor for loading silica, are urged at 60 DEG C~90 DEG C
Change reaction, products therefrom is collected after condensing, and obtains liquid sulfur dichloride.
Above-mentioned dichloride sulphur preparing process, it is preferred that the temperature of the synthetic reaction is 70 DEG C~90 DEG C.
Above-mentioned dichloride sulphur preparing process, it is preferred that the molar ratio of the chlorine and sulfur monochloride is 0.7~1.0:
1。
Above-mentioned dichloride sulphur preparing process, it is preferred that total reaction time is 6h~14h.
Above-mentioned dichloride sulphur preparing process, it is preferred that the partial size of the silica is 2 mm~5mm.
The inventive concept total as one, the present invention also provides used in a kind of above-mentioned dichloride sulphur preparing process
Preparation facilities, reaction solution kettle, catalytic reactor, condenser and reception kettle, the reaction solution kettle including being sequentially communicated are equipped with
Snorkel, the catalytic reactor include catalytic reaction tube and the heating tube that is sheathed on outside catalytic reaction tube, and the catalysis is reacted
Pipe both ends open, one end are connect with reaction solution kettle, and the other end is connect with condenser, and described heating tube one end enters equipped with heat medium
Mouthful, the other end is equipped with Crude product input.
Preparation facilities used in above-mentioned dichloride sulphur preparing process, it is preferred that the catalytic reactor is along vertical
Direction setting.
Preparation facilities used in above-mentioned dichloride sulphur preparing process, it is preferred that the condenser is close to reception kettle
One end be equipped with gas vent.
Compared with the prior art, the advantages of the present invention are as follows:
1, dichloride sulphur preparing process of the invention is taken due to the catalyst using silica as catalysis reaction
Obtained two unexpected technical effects: first is that synthesis two can be effectively suppressed as catalyst in silica at 60~90 DEG C
Reversible reaction in sulfur chloride, thus reaction conversion ratio is very high, sulfur dichloride yield reaches 92% or more.Second is that silica is
Granular solid-state, silica will not be dissolved into reaction product, thus gained sulfur dichloride product is remained without catalyst, nothing
It needs to distill, the purity is high of products obtained therefrom, up to 95% or more.
2, dichloride sulphur preparing process of the invention, synthetic reaction preferable temperature are 70 DEG C~90 DEG C, and applicant is through big
It is determined after amount experiment, the synthetic reaction of the temperature range reacts cooperation, gained sulfur dichloride product with 60 DEG C~90 DEG C of catalysis
High income.
3, the molar ratio of dichloride sulphur preparing process of the invention, chlorine and sulfur monochloride is preferably 0.7~1.0: 1,
The theoretical molar ratio of chlorine and sulfur monochloride synthesis sulfur dichloride is 0.5: 1, and the present invention increases the use of chlorine to a certain extent
Amount can be very good to inhibit sulfur dichloride to be decomposed into the back reaction of sulfur monochloride, the back reaction especially in catalytic reaction tube,
Improve the yield and quality of sulfur dichloride.
4, preparation facilities used in dichloride sulphur preparing process of the invention, easy to operate, continuous-stable are excessive
Chlorine is recycled；The waste that no exhaust gas, waste residue and waste liquid etc. pollute environment generates.Catalytic reactor is preferably along vertical side
To setting, though with the presence of sulfur monochloride in catalytic reaction products, since the boiling point of sulfur monochloride is 137 DEG C, and it is of the invention
Catalytic temperature is 60 DEG C~90 DEG C, and the inner wall for condensing into liquid runs down catalytic reaction tube is flowed back to reaction solution kettle by sulfur monochloride.Into
One step improves the purity of product.
Detailed description of the invention
Fig. 1 is preparation facilities used in the sulfur dichloride preparation method of the embodiment of the present invention.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
Embodiment:
A kind of dichloride sulphur preparing process, using sulfur monochloride and chlorine as raw material 60 DEG C~120 DEG C at a temperature of into
Row synthetic reaction, resulting gaseous mixture enter the catalytic reactor for loading silica, are urged at 60 DEG C~90 DEG C
Change reaction, products therefrom is collected after condensing, and obtains liquid sulfur dichloride.
Wherein, the molar ratio of chlorine and sulfur monochloride is 0.7~1.0: 1, and the time of the overall reaction is 6h~14h.Two
The partial size of silica is 2 mm~5mm.
Preparation facilities used in above-mentioned sulfur dichloride preparation method, including be sequentially communicated reaction solution kettle 1, catalysis reaction
Device 3, condenser 4 and reception kettle 5, reaction solution kettle 1 are equipped with snorkel 2, and catalytic reactor 3 includes catalytic reaction tube 31 and is arranged
In the heating tube 32 outside catalytic reaction tube, 31 both ends open of catalytic reaction tube, one end is connect with reaction solution kettle 1, the other end with it is cold
Condenser 4 connects, and heating tube one end is equipped with heating medium inlet, and the other end is equipped with Crude product input.
In the present embodiment, catalytic reactor 3 is arranged along the vertical direction；Condenser 4 is equipped with gas close to the one end for receiving kettle 5
Outlet 41.
The process of sulfur dichloride is prepared using the device are as follows: sulfur monochloride is added in reaction solution kettle 1, catalyst silica
Be packed into catalytic reaction tube, be passed through 60 DEG C~90 DEG C of circulation heat insulation liquid in heating tube 32, reaction solution kettle 1 be heated to 60 DEG C~
Chlorine is passed through after 120 DEG C, the temperature of reaction solution kettle 1 remains unchanged in reaction process, the gas phase portion warp at 3 top of catalytic reactor
Condenser 4 condense after enter receive kettle 5 in get arrive liquid sulfur dichloride.One directly is added to reaction solution kettle 1 after the reaction was completed
Sulfur chloride starts lower batch reaction.Uncooled gas (i.e. chlorine) escapes through gas vent 41, and being recycled after collection makes
With.
Embodiment 1:
110.00 g(1.63 mol are added into reaction solution kettle 1) sulfur monochloride, the silica loading of 40g partial size 2mm
Internal diameter is that 65 DEG C of liquid circulation heat preservations are passed through in heating tube 32 in the catalytic reaction tube 31 of 20mm, and reaction solution kettle 1 is heated to 120
Chlorine is passed through after DEG C, reaction kettle 1 maintains to stop logical chlorine, common 88.00 g(1.24 of chlorine after reacting 6 hours at such a temperature
Mol).The gas phase portion at 3 top of catalytic reactor obtains 160.93 g of sulfur dichloride product after the condensation of condenser 4, and product contains
Amount 97%, product yield 93%.Uncooled gas can be recycled after the collection of gas vent 41.
Embodiment 2:
110.00 g(1.63 mol are added into reaction solution kettle 1) sulfur monochloride, the silica dress of 40 g partial size, 5 mm
Enter in the catalytic reaction tube 31 that internal diameter is 20 mm, 65 DEG C of liquid circulation heat preservations are passed through in heating tube 32, reaction solution kettle 1 is heated to
Chlorine is passed through after 110 DEG C, reaction kettle 1 maintains to stop logical chlorine, common 88.00 g(1.24 of chlorine after reacting 14 hours at such a temperature
Mol).The gas phase portion at 3 top of catalytic reactor obtains 160.86 g of sulfur dichloride product after the condensation of condenser 4, and product contains
Amount 96%, product yield 92%.Uncooled gas can be recycled after the collection of gas vent 41.
Embodiment 3:
110 g(1.63 mol are added into reaction solution kettle 1) sulfur monochloride, in the silica of 70 g partial size, 3 mm is packed into
Diameter is that 60 DEG C of liquid circulation heat preservations are passed through in heating tube 32 in the catalytic reaction tube 31 of 20 mm, and reaction solution kettle 1 is heated to 90 DEG C
After be passed through chlorine, stop logical chlorine, common 115.70 g(1.63 mol of chlorine after reaction 13 hours).The gas at 3 top of catalytic reactor
Mutually part obtains 157.58 g of sulfur dichloride product, product content 98%, product yield 92% after the condensation of condenser 4.It is uncooled
Gas gas vent 41 collection after can be recycled.
Embodiment 4:
110.00 g(1.63 mol are added into reaction solution kettle 1) sulfur monochloride, the silica loading of 30g partial size 3mm
Internal diameter is that 90 DEG C of liquid circulation heat preservations are passed through in heating tube 32 in the catalytic reaction tube 31 of 20mm, and reaction solution kettle 1 is heated to 60 DEG C
After be passed through chlorine, reaction kettle 1 maintains to stop logical chlorine, common chlorine 81.01g(1.14 mol after reacting 13 hours at such a temperature).
The gas phase portion at the top of catalytic reactor 3 obtains 166.09 g of sulfur dichloride product after the condensation of condenser 4, product content 95%,
Product yield 94%.Uncooled gas can be recycled after the collection of gas vent 41.
Embodiment 5:
110.00 g(1.63 mol are added into reaction solution kettle 1) sulfur monochloride, the silica loading of 40g partial size 3mm
Internal diameter is that 65 DEG C of liquid circulation heat preservations are passed through in heating tube 32 in the catalytic reaction tube 31 of 20 mm, and reaction solution kettle 1 is heated to 70
Chlorine is passed through after DEG C, reaction kettle 1 maintains to stop logical chlorine, common 88.00 g(1.24 of chlorine after reacting 10 hours at such a temperature
Mol).The gas phase portion at 3 top of catalytic reactor obtains 169.62 g of sulfur dichloride product after the condensation of condenser 4, and product contains
Amount 95%, product yield 96%.Uncooled gas can be recycled after the collection of gas vent 41.Reaction solution kettle is directly used in down
One batch feeds intake.
Embodiment 6:
110.00 g(1.63 mol are added in reaction solution kettle 1 after having reacted to embodiment 5) sulfur monochloride, 40g partial size
The silica of 3mm is fitted into the catalytic reaction tube 31 that internal diameter is 20 mm, and 65 DEG C of liquid circulation heat preservations are passed through in heating tube 32,
Reaction solution kettle 1 is passed through chlorine after being heated to 85 DEG C, reaction kettle 1 maintains to stop logical chlorine after reacting 10 hours at such a temperature, common
88.00 g(1.24 mol of chlorine).The gas phase portion at 3 top of catalytic reactor obtains sulfur dichloride product after the condensation of condenser 4
174.92 g, product content 95%, product yield 99%.Uncooled gas can be recycled after the collection of gas vent 41.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example.All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It is noted that for the art
Those of ordinary skill for, improvements and modifications without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of dichloride sulphur preparing process, which is characterized in that using sulfur monochloride and chlorine be raw material at 60 DEG C~120 DEG C
At a temperature of carry out synthetic reaction, resulting gaseous mixture enters the catalytic reactor for loading silica, at 60 DEG C~90 DEG C
Under carry out catalysis reaction, products therefrom is collected after condensing, and obtains liquid sulfur dichloride.
2. dichloride sulphur preparing process according to claim 1, which is characterized in that the temperature of the synthetic reaction is 70
DEG C~90 DEG C.
3. dichloride sulphur preparing process according to claim 1, which is characterized in that the chlorine and sulfur monochloride rub
You are than being 0.7~1.0: 1.
4. dichloride sulphur preparing process according to claim 1, which is characterized in that total reaction time is 6h~14h.
5. dichloride sulphur preparing process according to claim 1, which is characterized in that the partial size of the silica is 2
Mm~5mm.
6. preparation facilities used in a kind of dichloride sulphur preparing process as claimed in any one of claims 1 to 5, feature
It is, including reaction solution kettle (1), catalytic reactor (3), condenser (4) and reception kettle (5) being sequentially communicated, the reaction solution
Kettle (1) is equipped with snorkel (2), and the catalytic reactor (3) includes catalytic reaction tube (31) and is sheathed on catalytic reaction tube
(31) outside heating tube (32), catalytic reaction tube (31) both ends open, one end are connect with reaction solution kettle (1), the other end with
Condenser (4) connection, described heating tube (32) one end are equipped with heating medium inlet, and the other end is equipped with Crude product input.
7. preparation facilities used in dichloride sulphur preparing process according to claim 6, which is characterized in that described to urge
Change reactor (3) to be arranged along the vertical direction.
8. preparation facilities used in dichloride sulphur preparing process according to claim 6 or 7, which is characterized in that institute
It states condenser (4) and is equipped with gas vent (41) close to the one end for receiving kettle (5).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3219413A (en) * | 1961-10-13 | 1965-11-23 | Hooker Chemical Corp | Process for production of sulfur dichloride |
| CN1473758A (en) * | 2003-06-26 | 2004-02-11 | 淄博市新材料研究所 | Method for preparing sulfur dichloride |
| CN104098072A (en) * | 2014-07-14 | 2014-10-15 | 湖南海利常德农药化工有限公司 | Preparation method for synthetizing sulfur dichloride through gas phase catalysis |
| CN106185809A (en) * | 2016-07-04 | 2016-12-07 | 汇智工程科技有限公司 | The method and device that in the production of a kind of thionyl chloride, chlorine efficiently utilizes |
-
2016
- 2016-12-20 CN CN201611182523.8A patent/CN106829878B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3219413A (en) * | 1961-10-13 | 1965-11-23 | Hooker Chemical Corp | Process for production of sulfur dichloride |
| CN1473758A (en) * | 2003-06-26 | 2004-02-11 | 淄博市新材料研究所 | Method for preparing sulfur dichloride |
| CN104098072A (en) * | 2014-07-14 | 2014-10-15 | 湖南海利常德农药化工有限公司 | Preparation method for synthetizing sulfur dichloride through gas phase catalysis |
| CN106185809A (en) * | 2016-07-04 | 2016-12-07 | 汇智工程科技有限公司 | The method and device that in the production of a kind of thionyl chloride, chlorine efficiently utilizes |
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Application publication date: 20170613 Assignee: Ningxia Haili Technology Co.,Ltd. Assignor: HUNAN HAILI CHANGDE PESTICIDE & CHEMICAL INDUSTRY CO.,LTD. Contract record no.: X2023980037360 Denomination of invention: Preparation method and device of Sulfur dichloride Granted publication date: 20190104 License type: Common License Record date: 20230703 |
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Inventor after: Hu Zhibin Inventor after: Feng Jiaolong Inventor after: Liu Weidong Inventor after: Zeng Xueyun Inventor after: Xu Jianbing Inventor after: Zhao Dongjiang Inventor after: Zeng Jing Inventor after: Chen Ming Inventor after: Xu Shibing Inventor after: Peng Changchun Inventor before: Hu Zhibin Inventor before: Zeng Xueyun Inventor before: Xu Jianbing Inventor before: Zhao Dongjiang Inventor before: Zeng Jing Inventor before: Chen Ming |
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