CN101254907A - Method for preparing phosphorus oxytrichloride - Google Patents
Method for preparing phosphorus oxytrichloride Download PDFInfo
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- CN101254907A CN101254907A CNA2008100199927A CN200810019992A CN101254907A CN 101254907 A CN101254907 A CN 101254907A CN A2008100199927 A CNA2008100199927 A CN A2008100199927A CN 200810019992 A CN200810019992 A CN 200810019992A CN 101254907 A CN101254907 A CN 101254907A
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- phosphorus oxychloride
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- oxygen
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Abstract
The invention relates to a method for preparing chemical material, particularly a method for preparing phosphorus oxychloride as the organic synthetic catalyst. The method is characterized in that three reaction kettles are used as reaction containers, one is used as a major reaction kettle, and the rest two are used as a minor reaction kettle and a second minor reaction kettle; after the reaction is completed in the major reaction kettle, and the reacted material is recovered, material in the minor reaction kettle is poured into the major reaction kettle, material in the second minor reaction kettle is poured into the minor reaction kettle, and phosphorous trichloride is fed into the second minor reaction kettle; unreacted oxygen in the major reaction kettle is introduced into the minor reaction kettle; and the unreacted oxygen in the minor reaction kettle is introduced into the second minor reaction kettle; two low-boiling kettles are disposed at the processing end to completely react the unreacted oxygen; and after reaction is completed, the reactant is distilled through a high efficiency packing tower to obtain phosphorus oxychloride product with good quality.
Description
Technical field
The present invention relates to a kind of method for preparing industrial chemicals, particularly prepare a kind of method of organic catalyst compound phosphorus oxychloride.
Background technology
Phosphorus oxychloride can be used as chlorizating agent, organic catalyst compound in chemical industry, purposes is very extensive, be one of main raw material of phosphoric acid ester organic products, be mainly used in industrial being widely used such as agricultural chemicals, pharmacy, dyestuff intermediate, semiconductor doping source and optical fiber material.In recent years, the development of the pesticide industry of China was swift and violent, and not only new product emerges in an endless stream like rain the back spring bamboo, and its output also increases rapidly.In these agricultural chemicals, is no lack of the kind of using phosphorus oxychloride, extensive as using future on the acetamide-group herbicides such as alachlor, acetochlor, the third careless amine, Butachlor technical 92, propachlor, ethaprochlor, prynachlor, delachlor, acetyl methoxalyl, terbuchlor, and use arranged also on quizalofopethyl, quizalofopPethyl, the production of China's phosphorus oxychloride starts from the fifties, all adopts phosphorus trichloride to drip basically and leads to the chlorine method.This method is with 4: 1 ratio the chlorine G﹠W to be fed in the phosphorus trichloride liquid phase, and its reaction formula is as follows:
PCl
3+CI
2——PCl
5
PCl
5+H
2O——POCl
3+2HCl
Emit a large amount of heats simultaneously.Its net reaction is:
PCl
3+ CI
2+ H
2O---POCl
3+ 2HCl+144.1 kilocalorie
Main consumption indicators is (a ton/ton):
PCl
3(98.5％) 1.04
Liquid chlorine (99.5%) 0.47
This method consumes height, the three wastes are many, reaction time is long, poor stability, and productivity levels is low.
Enter the nineties, some universities and colleges of China have begun the technical study of phosphorus trichloride dioxygen oxidation method production phosphorus oxychloride, Qingdao Organic Chemical Plant adopted this technology to build up 1000 tons of/year phosphorus oxychloride production equipments in 1991, and China's phosphorus oxychloride production level is improved.Phosphorus trichloride dioxygen oxidation method technology, phosphorus trichloride dioxygen oxidation method are methods comparatively advanced in the present phosphorus oxychloride production method.Its reaction formula is:
2PCI
3+O
2——2POCl
3
Phosphorus trichloride dioxygen oxidation method can be divided into again:
Vapour phase oxidation process
Vapour phase oxidation process is exactly that phosphorus trichloride gasification and oxygen are mixed with the reaction quantitative relation, feeds burner combustion then, and condensation just gets phosphorus oxychloride.
Vapour phase oxidation process can be made catalyzer with metal objects such as vanadium, molybdenum, chromium, manganese, and the gas composition of phosphorus trichloride and oxygen is controlled at beyond the limits of explosion, makes it to carry out the catalytic Contact oxidation.This method speed of response is fast, but to the equipment requirements height.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art part, a kind of method for preparing phosphorus oxychloride is provided, characteristics are with three reactors as reaction vessel, one of them is the main reaction still, all the other are secondary response still, secondary reaction still, after the main reaction still reacts completely rewinding the material in the secondary response still is ploughed under the main reaction still, the material in the secondary reaction still ploughs under the secondary response still, squeezes into phosphorus trichloride again in the secondary reaction still.Feed the feeding secondary response still that the oxygen in the main reaction still has not reacted, the oxygen that has not reacted in the secondary response still feeds the secondary reaction still.Add two low pots that boil that fill phosphorus trichloride then at the technology end, be intended to make the oxygen that has not reacted fully to react, reaction is distilled reactant after finishing through high efficiency packing tower, promptly get the excellent product of phosphorus oxychloride.
The objective of the invention is to realize: a kind of method for preparing phosphorus oxychloride with following technical scheme, it is characterized in that liquid phase phosphorus trichloride and gas phase oxygen successive reaction and make the product phosphorus oxychloride, described method reactor is three reactors, one of them is the main reaction still, all the other are the secondary response still, the secondary reaction still, concrete reaction process is: after the main reaction still has turned over material, the secondary response still ploughs under the main reaction still, the secondary reaction still ploughs under the secondary response still, the secondary reaction still is squeezed into phosphorus trichloride and is reacted, feed the feeding secondary response still that the oxygen in the main reaction still has not reacted, the oxygen that has not reacted in the secondary response still feeds the secondary reaction still, add two low pots that boil that fill phosphorus trichloride then at the technology end, be intended to make the oxygen that has not reacted fully to react.
The described method for preparing phosphorus oxychloride is characterized in that ratio of components (PCL3: O2): 1: 0.13.
The described method for preparing phosphorus oxychloride is characterized in that temperature of reaction is 67 ℃～90 ℃, and pressure is 100mmHg～150mmHg.
The described method for preparing phosphorus oxychloride is characterized in that solvent is a phosphorus trichloride.
The described method for preparing phosphorus oxychloride is characterized in that entering the rectifying separation system after the reaction mixture successive reaction, and reaction and rectifying have constituted continuous system.
Described method is characterized in that liquid oxygen need enter reactive system through vaporizer.
Described method is characterized in that logical oxygen speed: 5～15M3/h.
Described method is characterized in that logical oxygen pressure: 0.2Mpa～0.4Mpa.
Described method is characterized in that distillation collection temperature: 105 ℃～109 ℃.
Advantage of the present invention is: phosphorus trichloride dioxygen oxidation method is compared with other method, and advantage is fairly obvious, and this method operational path is reasonable, and reacting balance is easy to control, and raw material is easy to get, and cost is low, thereby favorable economic benefit is arranged.Good product quality reacts completely, the yield height, and three-waste free discharge helps protecting environment, and reaction process is simple, helps the realization of continuous process, especially compares with synthesis under normal pressure, and shorten reaction time greatly.
Description of drawings
The invention will be further described to reaching embodiment below in conjunction with accompanying drawing
Accompanying drawing is a process flow sheet of the present invention:
Among the figure: 1. phosphorus oxychloride storage tank, 2. still kettle, 3. dnockout pump, 4. phosphorus oxychloride storage tank, 5. phosphorus trichloride storage tank, 6. main reaction still, 7. secondary response still, 8. secondary reaction still, 9. liquid oxygen storage tank, 10. interchanger, 11. condensers, 12. rectifying tower, 13. the low pot that boils, 14. condensers, the 15. low pots that boil, 16. film-falling absorption tower, 17. hydrochloric acid tanks, 18. hydrochloric acid tanks, 19. hydrochloric acid tank, 24. vacuum pumps, 26. gas rotameters
Embodiment
A kind of method for preparing phosphorus oxychloride, it is characterized in that liquid phase phosphorus trichloride and gas phase oxygen successive reaction and make the product phosphorus oxychloride, described method reactor is three reactors, one of them is a main reaction still 6, all the other are secondary response still 7, secondary reaction still 8, concrete reaction process is: after main reaction still 6 has turned over material, secondary response still 7 ploughs under main reaction still 6, secondary reaction still 8 ploughs under secondary response still 7, secondary reaction still 8 is squeezed into phosphorus trichloride and is reacted, feed the feeding secondary response still 7 that the oxygen in the main reaction still 6 has not reacted, the oxygen that has not reacted in the secondary response still 7 feeds secondary reaction still 8, add two low pots 13 that boil that fill phosphorus trichloride then at the technology end, the low pot 15 that boils is intended to make the oxygen that has not reacted fully to react.
The described method for preparing phosphorus oxychloride is characterized in that ratio of components (PCL3: O2): 1: 0.13.
The described method for preparing phosphorus oxychloride is characterized in that temperature of reaction is 67 ℃, and pressure is 100mmHg.
The described method for preparing phosphorus oxychloride is characterized in that solvent is a phosphorus trichloride.
The described method for preparing phosphorus oxychloride is characterized in that entering the rectifying separation system after the reaction mixture successive reaction, and reaction and rectifying have constituted continuous system.
The described method for preparing phosphorus oxychloride is characterized in that liquid oxygen need enter reactive system through vaporizer.
The described method for preparing phosphorus oxychloride is characterized in that logical oxygen speed: 10M3/h.
The described method for preparing phosphorus oxychloride is characterized in that logical oxygen pressure: 0.3Mpa.
The described method for preparing phosphorus oxychloride is characterized in that distillation collection temperature: 105 ℃.
A kind of method for preparing phosphorus oxychloride, it is characterized in that liquid phase phosphorus trichloride and gas phase oxygen successive reaction and make the product phosphorus oxychloride, described method reactor is three reactors, one of them is a main reaction still 6, all the other are secondary response still 7, secondary reaction still 8, concrete reaction process is: after main reaction still 6 has turned over material, secondary response still 7 ploughs under main reaction still 6, secondary reaction still 8 ploughs under secondary response still 7, secondary reaction still 8 is squeezed into phosphorus trichloride and is reacted, feed the feeding secondary response still 7 that the oxygen in the main reaction still 6 has not reacted, the oxygen that has not reacted in the secondary response still 7 feeds secondary reaction still 8, add two low pots 13 that boil that fill phosphorus trichloride then at the technology end, the low pot 15 that boils is intended to make the oxygen that has not reacted fully to react.
The described method for preparing phosphorus oxychloride is characterized in that ratio of components (PCL3: O2): 1: 0.13.
The described method for preparing phosphorus oxychloride is characterized in that temperature of reaction is 90 ℃, and pressure is 150mmHg.
The described method for preparing phosphorus oxychloride is characterized in that solvent is a phosphorus trichloride.
The described method for preparing phosphorus oxychloride is characterized in that entering the rectifying separation system after the reaction mixture successive reaction, and reaction and rectifying have constituted continuous system.
The described method for preparing phosphorus oxychloride is characterized in that liquid oxygen need enter reactive system through vaporizer.
The described method for preparing phosphorus oxychloride is characterized in that logical oxygen speed: 15M3/h.
The described method for preparing phosphorus oxychloride is characterized in that logical oxygen pressure: 0.4Mpa.
The described method for preparing phosphorus oxychloride is characterized in that distillation collection temperature: 109 ℃.
Claims (9)
1, a kind of method for preparing phosphorus oxychloride, it is characterized in that liquid phase phosphorus trichloride and gas phase oxygen successive reaction and make the product phosphorus oxychloride, described method reactor is three reactors, one of them is a main reaction still (6), all the other are secondary response still (7), secondary reaction still (8), concrete reaction process is: after main reaction still (6) has turned over material, secondary response still (7) ploughs under main reaction still (6), secondary reaction still (8) ploughs under secondary response still (7), secondary reaction still (8) is squeezed into phosphorus trichloride and is reacted, feed the feeding secondary response still (7) that the oxygen in the main reaction still (6) has not reacted, the oxygen that has not reacted in the secondary response still (7) feeds secondary reaction still (8), add two low pots (13) that boil that fill phosphorus trichloride then at the technology end, (15), be intended to make the oxygen that has not reacted fully to react.
2. the method for preparing phosphorus oxychloride according to claim 1 is characterized in that ratio of components (PCL3: O2): 1: 0.13.
3, according to claim 1, the 2 described methods that prepare phosphorus oxychloride, it is characterized in that temperature of reaction is 67 ℃～90 ℃, pressure is 100mmHg～150mmHg.
4. according to claim 1, the 2 described methods that prepare phosphorus oxychloride, it is characterized in that solvent is a phosphorus trichloride.
5. according to claim 1, the 2 described methods that prepare phosphorus oxychloride, it is characterized in that entering the rectifying separation system after the reaction mixture successive reaction, and reaction and rectifying have constituted continuous system.
6,, it is characterized in that liquid oxygen need enter reactive system through vaporizer according to claim 1, the 2 described methods that prepare phosphorus oxychloride.
7,, it is characterized in that logical oxygen speed: 5～15M3/h according to claim 1, the 2 described methods that prepare phosphorus oxychloride.
8,, it is characterized in that logical oxygen pressure: 0.2Mpa～0.4Mpa according to claim 1, the 2 described methods that prepare phosphorus oxychloride.
9,, it is characterized in that distillation collection temperature: 105 ℃～109 ℃ according to claim 1, the 2 described methods that prepare phosphorus oxychloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100199927A CN101254907A (en) | 2008-03-18 | 2008-03-18 | Method for preparing phosphorus oxytrichloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100199927A CN101254907A (en) | 2008-03-18 | 2008-03-18 | Method for preparing phosphorus oxytrichloride |
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| Publication Number | Publication Date |
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| CN101254907A true CN101254907A (en) | 2008-09-03 |
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495115A (en) * | 2016-02-01 | 2017-03-15 | 江西电化乐丰化工股份有限公司 | A kind of process units of phosphorus oxychloride and production method |
-
2008
- 2008-03-18 CN CNA2008100199927A patent/CN101254907A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495115A (en) * | 2016-02-01 | 2017-03-15 | 江西电化乐丰化工股份有限公司 | A kind of process units of phosphorus oxychloride and production method |
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Open date: 20080903 |