CN106586989B - A method of cleaning phosphorus thiochloride reaction kettle - Google Patents
A method of cleaning phosphorus thiochloride reaction kettle Download PDFInfo
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- CN106586989B CN106586989B CN201611052619.2A CN201611052619A CN106586989B CN 106586989 B CN106586989 B CN 106586989B CN 201611052619 A CN201611052619 A CN 201611052619A CN 106586989 B CN106586989 B CN 106586989B
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/14—Sulfur, selenium, or tellurium compounds of phosphorus
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Abstract
The present invention provides a kind of methods for clearing up phosphorus thiochloride reaction kettle, it is characterised in that: (1) consumes sulphur in reaction kettle by the way that phosphorus trichloride is added dropwise, total reflux reaction is used when reacting；(2) after sulfur reaction is complete, mixture in reaction kettle is directly cooled to 70-75 DEG C, it is separated by solid-liquid separation after mixture in reaction kettle is discharged from reaction kettle bottom valve again, gained filtrate enters mother liquor tank after cooler is cooling, and it is dry that gained solid slag enters drying machine；When dry using drying machine, gained gas enters mother liquor tank after condensing, and the solid slag after gained is dry is sent into incinerator and is burned.The invention has the advantages that the step of present invention eliminates reaction solution in evaporation reaction kettle and adds water, avoids because residue is sticky, phosphorus trichloride, phosphorus thiochloride is caused unevenly to react with water generation, and then generate accumulation reaction and cause slug accident.The present invention can reduce security risk, improve utilization rate of equipment and installations, improve environment.
Description
Technical field
The present invention relates to technical field of waste water processing in Chemical Manufacture, and in particular to a kind of cleaning phosphorus thiochloride reaction kettle
Method.
Background technique
Phosphorus thiochloride is colourless or pale yellowish oil liquid, irritant smell, mainly as the raw material of manufacture pesticide.Three
Chlorothion has strong impulse effect to eyes, skin, mucous membrane and respiratory tract, and sucking is taken in or absorbed through skin to body
It is harmful.
Phosphorus thiochloride is the intermediate of pesticide orthene, is all made of semi-continuous production method at present.I.e. first anti-
It answers in kettle and puts into mother liquor (phosphorus thiochloride), be warming up to reflux, then put into sulphur, catalyst aluminium, maintain the reflux for state, be then added dropwise
Phosphorus trichloride fetches stream sample analysis, stops reflux after qualified, out product.When temperature is begun to decline, a batch reaction terminates.It will
Discharging is changed to flow back, and throws sulphur, catalyst aluminium again, starts next batch reaction.After repeating certain batch in this way, meeting in reaction kettle
Accumulate some residues, influence normally to produce, needs to carry out the waste residue in cleaning reaction kettle.
With the current prior art, the method for clearing up reaction kettle is: first passing through plus phosphorus trichloride consumes residue in reaction kettle
Sulphur (is commonly called as " eating " bottom sulphur), then steams reaction solution in reaction kettle, and the cooling when no liquid steams adds water to carry out cleaning reaction
Kettle.There are problems following prominent for this method:
(1) when adding water, because residue is sticky, wherein phosphorus trichloride, phosphorus thiochloride are reacted with the uneven of water, are easy accumulation
It reacts and slug accident occurs, security risk is larger.
(2) plus after water phosphorus trichloride, phosphorus thiochloride hydrolysis generation strong acid be will lead to, the loss of useful material is not only brought,
And corrosion equipment.
(3) H can be generated when adding water2S tail gas, need to be absorbed as the waste water of Containing Sulfur sodium with lye, and a pot waste water is washed in generation
Contain H2S, HCl, phosphorous acid, phosphoric acid, phosphite, phosphate etc., first is that increasing wastewater treatment difficulty, second is that discharge reaction kettle
When interior waste water, live smell is big, and environment is poor.
Therefore, a kind of method for being badly in need of inventing effective cleaning phosphorus thiochloride reaction kettle that can be safe and environment-friendly on Vehicles Collected from Market,
The method of this cleaning reaction kettle is significant to the production of phosphorus thiochloride.
Summary of the invention
It is an object of the invention in view of the above shortcomings of the prior art, provide a kind of side for clearing up phosphorus thiochloride reaction kettle
Method.The safe and environment-friendly residue removed in phosphorus thiochloride reaction kettle of this method energy, reduces security risk, reduces accident, subtract
The rare loss with material improves utilization rate of equipment and installations, reduces wastewater treatment difficulty, reduces smell, improves environment.
To achieve the goals above, the present invention adopts the following technical scheme:
A method of cleaning phosphorus thiochloride reaction kettle, it is characterised in that:
(1) sulphur in reaction kettle is consumed by the way that phosphorus trichloride is added dropwise, total reflux reaction is used when reacting；
(2) after sulfur reaction is complete, mixture in reaction kettle is directly cooled to 70-75 DEG C, then will mix in reaction kettle
Object is separated by solid-liquid separation after being discharged from reaction kettle bottom valve, and gained filtrate enters mother liquor tank, gained solid slag after cooler is cooling
It is dry into drying machine；When dry using drying machine, gained gas enters mother liquor tank, the solid slag after gained is dry after condensing
Incinerator is sent into burn.
Preferably, the reaction temperature of back flow reaction is 124 DEG C in the step (1), the reaction time is 1-1.5 hours.
Preferably, reaction kettle bottom valve uses extension upward type valve in the step (2).
Preferably, centrifuge or filter press can be used when being separated by solid-liquid separation in the step (2)；Carry out solid-liquid point
From when temperature be 50-100 DEG C；Double-cone type drying machine or vacuum rake dryer can be used in drying machine.
Further, preferably, centrifuge can be used when being separated by solid-liquid separation in the step (2)；Carry out solid-liquid
Temperature when separation is 70-75 DEG C；Vacuum rake dryer can be used in drying machine.
The beneficial effect that the present invention obtains is:
1, the present invention provides a kind of method for clearing up phosphorus thiochloride reaction kettle, this method compared with prior art, is removed
In evaporation reaction kettle reaction solution and plus the step of water, avoid because residue is sticky, phosphorus trichloride, phosphorus thiochloride and water caused to send out
Raw uneven reaction, and then generate accumulation reaction and cause slug accident.
2, the residue removed in phosphorus thiochloride reaction kettle that the method for the present invention can be safe and environment-friendly, reduces security risk, reduces
Accident occurs, and reduces the loss of useful material, improves utilization rate of equipment and installations, reduces wastewater treatment difficulty, reduces smell, improves ring
Border.
Specific embodiment
Introduced below is the specific embodiment of above content of the present invention, and by embodiment to foregoing teachings of the invention
Work further illustrates, but therefore the invention is limited to the scope of the described embodiments.
Embodiment 1:
(1) when needing to clear up reaction kettle, the consumption of 1300kg phosphorus trichloride is added dropwise in 3000L phosphorus thiochloride synthesis reaction vessel
Remaining sulphur in reaction kettle, the temperature control during phosphorus trichloride is added dropwise is 124 DEG C, maintains temperature after dropwise addition process
For 124 DEG C progress back flow reaction 1 hour；
(2) after sulfur reaction is complete, mixture in reaction kettle is directly cooled to 70-75 DEG C, then will mix in reaction kettle
Object is discharged from reaction kettle bottom valve and is put into centrifuge and is separated by solid-liquid separation, and gained filtrate enters mother liquor tank after cooler is cooling,
It is dry that gained solid slag enters drying machine；When dry using drying machine, gained gas enters mother liquor tank after condensing, and gained is dry
Solid slag afterwards is sent into incinerator and is burned.
Embodiment 2:
(1) when needing to clear up reaction kettle, the consumption of 1400kg phosphorus trichloride is added dropwise in 5000L phosphorus thiochloride synthesis reaction vessel
Remaining sulphur in reaction kettle, the temperature control during phosphorus trichloride is added dropwise is 124 DEG C, maintains temperature after dropwise addition process
For 124 DEG C progress back flow reaction 1.5 hours；
(2) after sulfur reaction is complete, mixture in reaction kettle is directly cooled to 50-55 DEG C, then will mix in reaction kettle
Object is discharged from reaction kettle bottom valve and is put into centrifuge and is separated by solid-liquid separation, and gained filtrate enters mother liquor tank after cooler is cooling,
It is dry that gained solid slag enters drying machine；When dry using drying machine, gained gas enters mother liquor tank after condensing, and gained is dry
Solid slag afterwards is sent into incinerator and is burned.
Embodiment 3
(1) when needing to clear up reaction kettle, the consumption of 1400kg phosphorus trichloride is added dropwise in 5000L phosphorus thiochloride synthesis reaction vessel
Remaining sulphur in reaction kettle, the temperature control during phosphorus trichloride is added dropwise is 124 DEG C, maintains temperature after dropwise addition process
For 124 DEG C progress back flow reaction 1.5 hours；
(2) after sulfur reaction is complete, mixture in reaction kettle is directly cooled to 90-95 DEG C, then will mix in reaction kettle
Object is discharged from reaction kettle bottom valve and is put into centrifuge and is separated by solid-liquid separation, and gained filtrate enters mother liquor tank after cooler is cooling,
It is dry that gained solid slag enters drying machine；When dry using drying machine, gained gas enters mother liquor tank after condensing, and gained is dry
Solid slag afterwards is sent into incinerator and is burned.
Claims (4)
1. a kind of method for clearing up phosphorus thiochloride reaction kettle, it is characterised in that:
(1) sulphur in reaction kettle is consumed by the way that phosphorus trichloride is added dropwise, total reflux reaction is used when reacting；
(2) after sulfur reaction is complete, mixture in reaction kettle is directly cooled to 70-75 DEG C, then by mixture in reaction kettle from
It is separated by solid-liquid separation after being discharged at reaction kettle bottom valve, gained filtrate enters mother liquor tank after cooler is cooling, and gained solid slag enters
Drying machine is dry；When dry using drying machine, gained gas enters mother liquor tank after condensing, and the solid slag after gained is dry is sent into
Incinerator burns；
In the step (1), the reaction temperature of back flow reaction is 124 DEG C, and the reaction time is 1-1.5 hours.
2. the method for cleaning phosphorus thiochloride reaction kettle according to claim 1, it is characterised in that: in the step (2), instead
Answer bottom valve using extension upward type valve.
3. the method for cleaning phosphorus thiochloride reaction kettle according to claim 1, it is characterised in that: in the step (2), into
Centrifuge or filter press can be used when being separated by solid-liquid separation in row；Temperature when being separated by solid-liquid separation is 50-100 DEG C；Drying machine can be used
Double-cone type drying machine or vacuum rake dryer.
4. the method for cleaning phosphorus thiochloride reaction kettle according to claim 1, it is characterised in that: in the step (2), into
Centrifuge can be used when being separated by solid-liquid separation in row；Temperature when being separated by solid-liquid separation is 70-75 DEG C；It is dry that vacuum rake type can be used in drying machine
Dry machine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611052619.2A CN106586989B (en) | 2016-11-25 | 2016-11-25 | A method of cleaning phosphorus thiochloride reaction kettle |
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| CN201611052619.2A CN106586989B (en) | 2016-11-25 | 2016-11-25 | A method of cleaning phosphorus thiochloride reaction kettle |
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| CN106586989A CN106586989A (en) | 2017-04-26 |
| CN106586989B true CN106586989B (en) | 2018-12-28 |
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| CN112320774B (en) * | 2020-09-07 | 2022-02-18 | 徐州市建平化工有限公司 | Production process for improving trichloro sulfur phosphorus yield |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6251350B1 (en) * | 1999-06-21 | 2001-06-26 | Bayer Corporation | Process for the manufacture of thiophosphoryl chloride |
| CN202924738U (en) * | 2012-10-12 | 2013-05-08 | 徐州江海源精细化工有限公司 | Novel device for producing thiophosphoryl chloride |
| CN104150454A (en) * | 2013-05-15 | 2014-11-19 | 新沂市汉菱生物工程有限公司 | Production method for thiophosphoryl chloride |
-
2016
- 2016-11-25 CN CN201611052619.2A patent/CN106586989B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6251350B1 (en) * | 1999-06-21 | 2001-06-26 | Bayer Corporation | Process for the manufacture of thiophosphoryl chloride |
| CN202924738U (en) * | 2012-10-12 | 2013-05-08 | 徐州江海源精细化工有限公司 | Novel device for producing thiophosphoryl chloride |
| CN104150454A (en) * | 2013-05-15 | 2014-11-19 | 新沂市汉菱生物工程有限公司 | Production method for thiophosphoryl chloride |
Non-Patent Citations (2)
| Title |
|---|
| 三氯硫磷清釜尾气的治理;石家庄市黄磷厂;《化工环保》;19921231;第12卷(第6期);367-368 * |
| 三氯硫磷清釜方法;刘延年;《农药》;19891231;第28卷(第4期);8-9 * |
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