CN102351681A - Method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride - Google Patents
Method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride Download PDFInfo
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Abstract
The invention relates to a method for continuously synthesizing trifluoroacetyl chloride and sulfuryl fluoride, which comprises the following process: continuously introducing sulfur trioxide and trifluorotrichloroethane (F113a) into a reaction rectifying tower containing a catalyst and a filler thorough the lower part in the tower according to a mol ratio of 1:1, wherein the temperature of the tower is controlled to range between 120 DEG C and 130 DEG C, and the reflux ratio at the top of the tower is 2.5-3; introducing tower bottoms into a sulfuryl chloride separating tower for rectification and separation, wherein the tower temperature is 145-150 DEG C, and the reflux ratio is 0.5-1.0; returning pyrosulfuryl chloride in the separating tower to the middle upper part of the reaction rectifying tower, heating the sulfuryl chloride rectified off from the top of the tower to 150 DEG C, and then introducing the rectified sulfuryl chloride and preheated recycled and newly-added hydrogen fluoride gas into a reactor containing a palladium/charcoal catalyst, wherein the reaction temperature is controlled to range between 150 DEG C and 160 DEG C; separating out unreacted hydrogen fluoride from the reaction product through a cold trap, and returning to the reactor for further use; and then absorbing and separating hydrogen chloride through a falling film, drying, compressing, and condensing to obtain the sulfuryl fluoride. The invention has the advantage of easy acquisition of raw materials, and the sulfuryl chloride byproduct can be directly used for the synthesis of sulfuryl fluoride.
Description
Technical field
The present invention relates to the method for a kind of continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride.
Background technology
Trifluoroacetyl chloride (CF
3COCl) containing the acid chloride groups of high reaction activity, can generate the trifluoroacetic acid derivative with the reaction of multiclass compound, is a kind of important fine-chemical intermediate.Sulfuryl fluoride (SO
2F
2) also be one type of important fine-chemical intermediate, can be used for synthetic perfluorochemical, it still is one type of good fumigant, is used for the Pesticidal and sterilizing of a plurality of industries.
According to bibliographical information, the synthesis method of trifluoroacetyl chloride mainly contains following several types.
First kind method is that Halothane muriate (mainly being that trifluorobichloroethane is that F123 and trifluoro monochlorethane are F133) reacts synthetic trifluoroacetyl chloride under certain condition with oxygen.
Document (Zhao Jianming, Han Zhenxian, Cui Juejian; " a kind of method for preparing trifluoroacetyl chloride by the Halothane chloride mix ", application number 200910156965.9, application publication number CN101747176A) and document (Zhao Jianming; Korea Spro admonishes virtuous; Cui Juejian, " a kind of by 2,2-two chloro-1; 1; the 1-Halothane prepares the method for trifluoroacetyl chloride ", application number 200910155786.3, application publication number CN101735033A.Zhao Jianming, Han Zhenxian, Cui Juejian, " a kind of preparation method of trifluoroacetyl chloride ", application number 200910155787.8, application publication number CN101735034A.) respectively with Halothane chlorinated mixture and 2; 2-two chloro-1; 1; The 1-Halothane is a raw material, under the mercury lamp radiation, carries out the photochemical oxidation reaction with oxygen, chlorine, and reaction yield is report not; But except the principal product trifluoroacetyl chloride, also has unstripped gas, oxygen, chlorine and hydrogenchloride in the gas-phase product of reaction; Form complicated, cause product to separate and raw material to apply mechanically difficulty bigger, be difficult to realize industrialization.
Document (Ning Dan; Huang Qing; Wu Yindeng; Zhu Jinzhi; Liu Chunshan, " gac prepares the application in the trifluoroacetyl chloride at the catalyzed oxidation trifluorobichloroethane ", Industrial Catalysis (2007); V15 (2): be that oxygen source, gac are that catalyzer prepares trifluoroacetyl chloride with the F123 oxidation with oxygen 62-64), reaction yield has only 71%.
US5296640 proposition oxidation F123 under supercritical state prepares trifluoroacetyl chloride, has by product hydrofluoric acid and trifluoroacetic acid to produce in the reaction, and reaction process needs High Temperature High Pressure, and product is easy to decompose, and also is difficult in the industry realize.
US5259938 carries out the photochemical oxidation prepared in reaction trifluoroacetyl chloride of F123 or F133 and oxygen under chlorine existence and mercury lamp radiation; Through using wavelength to improve the selectivity of reaction, must be pure F123 or F133 but this method requires reaction raw materials greater than the method for 280nm.
JP60239437 in the presence of water with F123 with oxygen at 300 ℃ and 30Kg/cm
2Following oxidation prepares trifluoroacetyl chloride, and reaction conversion ratio can reach 95%, but the selectivity of trifluoroacetyl chloride has only 26%.
US5241113 prepares trifluoroacetyl chloride with activated carbon catalysis F123 oxidation down at 200～325 ℃, and the temperature of reaction of this method is higher, is prone to cause reaction raw materials and product to decompose, and makes reaction preference and yield lower, does not have industrial value.
JP58159440 proposes to exist in less water, prepare trifluoroacetyl chloride with dioxygen oxidation F123 150～500 ℃ times, and reaction conversion ratio and selectivity are all lower, and industrial value is not high.
US5041647 makes and uses water as catalyst oxidation F123 and prepare trifluoroacetyl chloride, and the existence of water makes to be reflected at when generating product and also can produce trifluoroacetic acid, trifluoroacetyl chloride, trifluoroacetic acid and water separate very difficulty.
US5545298 prepares trifluoroacetyl chloride through gaseous oxidation F123 under higher reaction temperatures, product is easy to decompose under temperature of reaction, causes yield to descend the product separation difficulty.
US3883407 is less than 0.1% F123 through ultraviolet lamp radiation gaseous oxidation water content and prepares trifluoroacetyl chloride, and this method need just can be carried out under certain temperature and pressure, and the hydrofluoric acid that side reaction simultaneously generates can corrode ultraviolet lamp tube.Be not difficult to find out that the reaction conditions of oxidation style is comparatively harsh, is easy to produce side reaction, reaction yield is lower.
Second class methods are to be raw material with Freon 113 (F113a), under catalyst action and sulphur trioxide (SO
3) reaction generation trifluoroacetyl chloride.
JP60237040 has described when simple substance bromine exists, F113a and SO under the uv-radiation
3Reaction generates trifluoroacetyl chloride, and reaction yield can reach 90.1%, but when not having uv-radiation, reaction product does not almost have.
US4340548 proposes under halogen family simple substance or compound for catalysis, F113a and SO
3Reaction can generate trifluoroacetyl chloride, has only 84% but reaction conversion ratio is the highest, and product is formed complicated, and separation difficulty is unfavorable for industrialization.
DE2947376 is with BF
3Be catalyzer, with F113a and SO
3The prepared in reaction trifluoroacetyl chloride, reaction yield has only 80%.
It is when having sulfuryl chloride or pyrosulfuryl chloride to exist in composite catalyst, the system that DE1917630 and US3725475 have all described with sulfuric acid, Mercury bisulfate and mercurous sulfate, F113a and SO
3The method of prepared in reaction trifluoroacetyl chloride, reaction yield can reach 96%, but the catalyst system component of this method is more, the separation of the sulfuryl chloride of also not considering to generate in the reaction process and utilize problem.
JP56501649 adopts very complicated catalyst system (compositions such as mercury salt, boron halogenide and halogenosulfonic acid) catalysis F113a and SO
3Prepared in reaction trifluoroacetyl chloride, reaction yield be report not, but the catalyst system component of this method is more, the separation of the sulfuryl chloride of also not considering to generate in the reaction process and utilize problem.
Compare with oxidation style, the sulphur trioxide method can be carried out under lower temperature of reaction and normal pressure, but catalyst system is formed the separation of the sulfuryl chloride that produces in complicacy, the reaction process and it is to be solved to utilize problem also to have.
The 3rd class methods are methods of prepared in reaction trifluoroacetyl chloride such as hydrochloride such as the sodium-chlor of the described trifluoroacetic anhydride of DE4313793 and pyridine hydrochloride or metal, and reaction yield is report not, but the cost of material of this method is higher.
To be that DE2203326 is described take the trichoroacetic chloride as the synthetic trifluoroacetyl chloride of raw material two step method to the 4th class methods.Exist and CrO at simple substance chlorine
2F
2Under the catalysis, trichoroacetic chloride and hydrogen fluoride obtain Trifluoroacetyl fluoride 240 ℃ of reactions, add catalyzer CrO subsequently
2F
2, and tetracol phenixin joined in the Trifluoroacetyl fluoride, obtaining trifluoroacetyl chloride 220 ℃ of reactions, reaction yield is 73%.The catalytic amount that this method consumes is bigger, and raw material also is difficult to obtain, and reaction yield is not high, and industrial value is little.
According to bibliographical information, the synthesis method of sulfuryl fluoride then has following several.
US2879138 is with pyrosulfuryl fluorine (S
2O
5F
2) under temperature more than 200 ℃, carry out thermolysis and prepare sulfuryl fluoride, because temperature of reaction is higher, so can produce by product Thionyl difluoride (SOF in the reaction process
2) and sulfurous gas, cause reaction conversion ratio and selectivity not high, there is not industrial value.
US6238642B1 is under basic metal catalysis; With sulfurous gas and simple substance fluoride is the synthetic sulfuryl fluoride of raw material; React temperature required not high; But reaction conversion ratio is report not; Can generate multiple by products such as sulfur hexafluoride, Thionyl difluoride with the variation of reaction conditions in the reaction process, increase the product separating difficulty.
US4382072 is catalyzer, under 150～200 ℃, is the synthetic sulfuryl fluoride of raw material with sulfurous gas, simple substance chlorine and hydrogen fluoride that with the gac of appendix palladium metal though there is not the by product Thionyl difluoride to generate, reaction yield is less than 10%, and industrial value is not high.
US4003984 is catalyzer, under 125～400 ℃, is the synthetic sulfuryl fluoride of raw material with sulfurous gas, simple substance chlorine and hydrogen fluoride with the gac of appendix alkaline-earth metal fluoride, prolongs the reaction times can improve reaction yield.
US3497427 feeds electrolyzer with sulfurous gas and anhydrous hydrogen fluoride to carry out electrochemical reaction and prepares sulfuryl fluoride; Reaction yield can reach 90.4% in sulfurous gas under the helium protection; But this method needs the interior productive rate of helium and excessive anhydrous hydrogen fluoride and unit time not high, is unfavorable for industrialization.
US3687626 is with bifluoride hydrogen ammonium (NH
4HF
2) and sulfuryl chloride (SO
2Cl
2) be raw material at 90～150 ℃ of synthetic sulfuryl fluorides, reaction yield has only 59%, does not have industrial value.
US3146068 obtains the mixture of sulfuryl fluoride, silicon tetrafluoride and sulphur trioxide with Calcium Fluoride (Fluorspan) and sulphur trioxide 600～800 ℃ of reactions, and reaction conversion ratio is lower than 30%, and industrial value is little.
US3132925 with gas phase sulfur trioxide through being controlled to be 12～24 seconds Calcium Fluoride (Fluorspan), the duration of contact that is heated to 300～600 ℃; Obtain the mixture of sulfuryl fluoride, silicon tetrafluoride and sulfurous gas; Reaction yield is up to 85%, does not relate to the separation of by product silicon tetrafluoride.
US3107979 is catalyzer with the gac, under 125～600 ℃, with sulfurous gas and nitrosyl fluoride (NOF) or nitrosyl fluoride and hydrofluoric mixture (NOFHF), be the synthetic sulfuryl fluoride of raw material; Reaction yield has only 41%; In addition, raw materials used nitrosyl fluoride also is difficult for obtaining.US3092458 is catalyzer with the gac, under 230～240 ℃, be the synthetic sulfuryl fluoride of raw material with sulfurous gas, simple substance chlorine and hydrogen fluoride, reaction contact time is 1～11 second, reaction yield surpasses 80%, but the evaluation that does not relate to by product with separate.
At 500～650 ℃ of following prepared in reaction sulfuryl fluorides, reaction yield is not high, does not relate to the separation problem of by product silicon tetrafluoride yet with sulphur trioxide and barium fluoride or hexafluoro silicon barium for US3403144, and raw material barium fluoride of this method or hexafluoro silicon barium also are difficult for obtaining.
CN1259515 prepares sulfuryl fluoride by sulfurous gas and simple substance fluoride in the presence of alkaline metal fluoride cpd and hydrofluoric acid, reaction can be carried out at a lower temperature, but reaction product is formed complicacy, and reaction yield is report not, does not also relate to the separation problem of by product.
(happy will is strong for document; Bao Shengmin; Wang Guangjian; Inorganic fine chemicals handbook; Chemical Industry Press (2001); 344～345) be that raw material prepares sulfuryl fluoride through pyrolysis with fluosulfonic acid and anhydrous barium chloride in, the temperature of reaction of this method is high, sulfuryl fluoride be easy to decompose cause product form complicated, reaction yield is not high.
In sum, the method for existing synthetic trifluoroacetyl chloride and sulfuryl fluoride is synthetic separately, and by product is not separated utilization effectively, and therefore, production cost is high, and the three wastes are many.
Summary of the invention
The objective of the invention is to existing problem in the synthesis method of above-mentioned bibliographical information, the method for a kind of continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride is provided.
The step of the method for continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride is following:
1) sulphur trioxide of mol ratio 1:1 and Freon 113 are fed the reaction fractionating tower middle and lower part that catalyzer and filler are housed continuously, control tower still temperature is that 120～130 ℃, reflux ratio are 2.5～3, from cat head extraction trifluoroacetyl chloride;
2) sulfuryl chloride in the reaction fractionating tower still and pyrosulfuryl chloride are delivered to the sulfuryl chloride knockout tower and carry out rectifying separation, controlling this Tata still temperature and be 145～150 ℃, reflux ratio is 0.5～1.0, and the pyrosulfuryl chloride that separates in the Tata still returns to the reaction fractionating tower middle and upper part;
3) sulfuryl chloride is separated cat head distilled sulfuryl chloride and add the reactor that hydrogen fluoride gas is adorned Pd/carbon catalyst in getting into from the top with new through being heated to after 150 ℃ with the good recovery hydrogen fluoride of preheating; Control reaction temperature is 150～160 ℃; The cold-trap that the reaction product entering of outflow reactor is-40 ℃ is isolated unreacted hydrogen fluoride; Being circulated to reactor head through pump applies mechanically; Two film-falling absorption tower water absorption extraction of condensed reaction product entering go out hydrogenchloride becomes 30% hydrochloric acid, and aqueous sulfuryl fluoride gas is dry through drying tube again; Compression; Condensation obtains the sulfuryl fluoride product.
The catalyzer that loads in the said reaction fractionating tower is meant the perfluorosulfonic acid resin that has exchanged mercury salt and mercurous salt.The mol ratio of said new adding hydrogen fluoride and Freon 113 is 2:1.
Advantage of the present invention is: the main raw material Freon 113 (F113a) that is adopted is the by product in the F113 production process of fluorine Lyons, and is cheap and easy to get; In the trifluoroacetyl chloride building-up process sulphur trioxide need not excessive; Trifluoroacetyl chloride building-up reactions by product sulfuryl chloride can directly be used for the synthetic of sulfuryl fluoride after separating.Compare synthesis method reaction yield of the present invention with the bibliographical information method high, and the three wastes are few.
Description of drawings
Accompanying drawing is continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride process flow sheet.
Embodiment
The step of the method for continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride is following:
1) sulphur trioxide of mol ratio 1:1 and Freon 113 are fed the reaction fractionating tower middle and lower part that catalyzer and filler are housed continuously, control tower still temperature is that 120～130 ℃, reflux ratio are 2.5～3, from cat head extraction trifluoroacetyl chloride;
2) sulfuryl chloride in the reaction fractionating tower still and pyrosulfuryl chloride are delivered to the sulfuryl chloride knockout tower and carry out rectifying separation, controlling this Tata still temperature and be 145～150 ℃, reflux ratio is 0.5～1.0, and the pyrosulfuryl chloride that separates in the Tata still returns to the reaction fractionating tower middle and upper part;
3) sulfuryl chloride is separated cat head distilled sulfuryl chloride and add the reactor that hydrogen fluoride gas is adorned Pd/carbon catalyst in getting into from the top with new through being heated to after 150 ℃ with the good recovery hydrogen fluoride of preheating; Control reaction temperature is 150～160 ℃; The cold-trap that the reaction product entering of outflow reactor is-40 ℃ is isolated unreacted hydrogen fluoride; Being circulated to reactor head through pump applies mechanically; Two film-falling absorption tower water absorption extraction of condensed reaction product entering go out hydrogenchloride becomes 30% hydrochloric acid, and aqueous sulfuryl fluoride gas is dry through drying tube again; Compression; Condensation obtains the sulfuryl fluoride product.
The catalyzer that loads in the said reaction fractionating tower is meant the perfluorosulfonic acid resin that has exchanged mercury salt and mercurous salt.The mol ratio of said new adding hydrogen fluoride and Freon 113 is 2:1.
The present invention is that the reaction equation of synthetic trifluoroacetyl chloride of raw material and sulfuryl fluoride is following with F113a:
Below in conjunction with synthesizing trifluoroacetyl chloride and sulfuryl fluoride process flow sheet and embodiment continuously the present invention is described in detail.
Embodiment 1
1) with the Freon 113 (F113a) of 600 moles/hour sulphur trioxide and 600 moles/hour at the bottom of tower 500 millimeters locate to feed continuously reaction fractionating tower (diameter be that 50 millimeters, total height are 2000 millimeters; Tower middle part, bottom totally 1500 millimeters dresses be the perfluorosulfonic acid resin filler that has exchanged mercury salt and mercurous salt, the 500 millimeters dresses in top be the glass spring filler.) react, control tower still temperature is that 120 ℃, reflux ratio are 2.5, is 594 moles/hour from the amount of cat head extraction trifluoroacetyl chloride;
2) with the sulfuryl chloride in the reaction fractionating tower still and pyrosulfuryl chloride with pump send at 200 millimeters places at the bottom of tower the sulfuryl chloride knockout tower (diameter is 50 millimeters, and total height is 600 millimeters, interior glaze spring filler, its middle and upper part filler is 400 millimeters.) carry out rectifying separation, control tower still temperature is that 145 ℃, reflux ratio are 0.5, the pyrosulfuryl chloride in the knockout tower still circulates in apart from 500 millimeters places of cat head through pump and is back to reaction fractionating tower,
3) sulfuryl chloride being separated cat head distilled sulfuryl chloride gets into reactor with the good hydrogen fluoride gas of preheating (newly adding the hydrogen fluoride flow is 1200 moles/hour) (diameter is 125 millimeters through being heated to after 150 ℃ from the top; Height is 6000 millimeters, interior dress Pd/carbon catalyst.) react; Control reaction temperature is 150 ℃; Effusive reaction product gets into that condensation separation goes out unreacted hydrogen fluoride in-40 ℃ the cold-trap from reactor; Being circulated to reactor head through pump applies mechanically; Condensed reaction product gets into two film-falling absorption tower water absorption extraction hydrogenchloride becomes 30% hydrochloric acid; Aqueous sulfuryl fluoride gas obtains the sulfuryl fluoride product through drying tube drying, compression, condensation, and its flow is 582 moles/hour.
Embodiment 2
1) with the Freon 113 (F113a) of 600 moles/hour sulphur trioxide and 600 moles/hour at the bottom of tower 500 millimeters locate to feed continuously reaction fractionating tower (diameter be that 50 millimeters, total height are 2000 millimeters; Tower middle part, bottom totally 1500 millimeters dresses be the perfluorosulfonic acid resin filler that has exchanged mercury salt and mercurous salt, the 500 millimeters dresses in top be the glass spring filler.) react, control tower still temperature is that 130 ℃, reflux ratio are 3.0, is 597 moles/hour from the amount of cat head extraction trifluoroacetyl chloride;
2) with the sulfuryl chloride in the reaction fractionating tower still and pyrosulfuryl chloride with pump send at 200 millimeters places at the bottom of tower the sulfuryl chloride knockout tower (diameter is 50 millimeters, and total height is 600 millimeters, interior glaze spring filler, its middle and upper part filler is 400 millimeters.) carry out rectifying separation, control tower still temperature is that 150 ℃, reflux ratio are 1.0, the pyrosulfuryl chloride in the knockout tower still circulates in apart from 500 millimeters places of cat head through pump and is back to reaction fractionating tower;
3) sulfuryl chloride being separated cat head distilled sulfuryl chloride gets into reactor with the good hydrogen fluoride gas of preheating (newly adding the hydrogen fluoride flow is 1200 moles/hour) (diameter is 125 millimeters through being heated to after 150 ℃ from the top; Height is 6000 millimeters, interior dress Pd/carbon catalyst.) react; Control reaction temperature is 160 ℃; Effusive reaction product gets into that condensation separation goes out unreacted hydrogen fluoride in-40 ℃ the cold-trap from reactor; Being circulated to reactor head through pump applies mechanically; Condensed reaction product gets into two film-falling absorption tower water absorption extraction hydrogenchloride becomes 30% hydrochloric acid; Aqueous sulfuryl fluoride gas obtains the sulfuryl fluoride product through drying tube drying, compression, condensation, and its flow is 588 moles/hour.
Embodiment 3
1) with the Freon 113 (F113a) of 600 moles/hour sulphur trioxide and 600 moles/hour at the bottom of tower 500 millimeters locate to feed continuously reaction fractionating tower (diameter be that 50 millimeters, total height are 2000 millimeters; Tower middle part, bottom totally 1500 millimeters dresses be the perfluorosulfonic acid resin filler that has exchanged mercury salt and mercurous salt, the 500 millimeters dresses in top be the glass spring filler.) react, control tower still temperature is that 127 ℃, reflux ratio are 2.8, is 596 moles/hour from the amount of cat head extraction trifluoroacetyl chloride;
2) with the sulfuryl chloride in the reaction fractionating tower still and pyrosulfuryl chloride with pump send at 200 millimeters places at the bottom of tower the sulfuryl chloride knockout tower (diameter is 50 millimeters, and total height is 600 millimeters, interior glaze spring filler, its middle and upper part filler is 400 millimeters.) carry out rectifying separation, control tower still temperature is that 147 ℃, reflux ratio are 0.8, the pyrosulfuryl chloride in the knockout tower still circulates in apart from 500 millimeters places of cat head through pump and is back to reaction fractionating tower;
3) sulfuryl chloride being separated cat head distilled sulfuryl chloride gets into reactor with the good hydrogen fluoride gas of preheating (newly adding the hydrogen fluoride flow is 1200 moles/hour) (diameter is 125 millimeters through being heated to after 150 ℃ from the top; Height is 6000 millimeters, interior dress Pd/carbon catalyst.) react; Control reaction temperature is 155 ℃; Effusive reaction product gets into that condensation separation goes out unreacted hydrogen fluoride in-40 ℃ the cold-trap from reactor; Being circulated to reactor head through pump applies mechanically; Condensed reaction product gets into two film-falling absorption tower water absorption extraction hydrogenchloride becomes 30% hydrochloric acid; Aqueous sulfuryl fluoride gas obtains the sulfuryl fluoride product through drying tube drying, compression, condensation, and its flow is 585 moles/hour.
Claims (3)
1. the method for continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride is characterized in that its step is following:
1) sulphur trioxide of mol ratio 1:1 and Freon 113 are fed the reaction fractionating tower middle and lower part that catalyzer and filler are housed continuously, control tower still temperature is that 120～130 ℃, reflux ratio are 2.5～3, from cat head extraction trifluoroacetyl chloride;
2) sulfuryl chloride in the reaction fractionating tower still and pyrosulfuryl chloride are delivered to the sulfuryl chloride knockout tower and carry out rectifying separation, controlling this Tata still temperature and be 145～150 ℃, reflux ratio is 0.5～1.0, and the pyrosulfuryl chloride that separates in the Tata still returns to the reaction fractionating tower middle and upper part;
3) sulfuryl chloride is separated cat head distilled sulfuryl chloride and add the reactor that hydrogen fluoride gas is adorned Pd/carbon catalyst in getting into from the top with new through being heated to after 150 ℃ with the good recovery hydrogen fluoride of preheating; Control reaction temperature is 150～160 ℃; The cold-trap that the reaction product entering of outflow reactor is-40 ℃ is isolated unreacted hydrogen fluoride; Being circulated to reactor head through pump applies mechanically; Two film-falling absorption tower water absorption extraction of condensed reaction product entering go out hydrogenchloride becomes 30% hydrochloric acid, and aqueous sulfuryl fluoride gas is dry through drying tube again; Compression; Condensation obtains the sulfuryl fluoride product.
2. the method for a kind of continuously synthetic trifluoroacetyl chloride as claimed in claim 1 and sulfuryl fluoride is characterized in that the catalyzer that loads in the said reaction fractionating tower is meant the perfluorosulfonic acid resin that has exchanged mercury salt and mercurous salt.
3. the method for a kind of continuously synthetic trifluoroacetyl chloride as claimed in claim 1 and sulfuryl fluoride is characterized in that the mol ratio of said new adding hydrogen fluoride and Freon 113 is 2:1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104671219A (en) * | 2013-12-02 | 2015-06-03 | 浙江化工院科技有限公司 | Sulfuric chloride separation and purification technique |
| CN106946231A (en) * | 2017-03-30 | 2017-07-14 | 杭州茂宇电子化学有限公司 | A kind of method and system for producing high-purity vikane |
| CN109369385A (en) * | 2018-11-12 | 2019-02-22 | 江山鑫隆化工有限公司 | A kind of preparation method of Trifluoroacetic Acid Ethyl Ester |
| CN114368728A (en) * | 2022-01-29 | 2022-04-19 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride |
| WO2023142047A1 (en) * | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by electrofluorination |
| WO2023142027A1 (en) | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride |
| CN116812876A (en) * | 2023-07-14 | 2023-09-29 | 河南省氟基新材料科技有限公司 | Preparation method of sulfuryl fluoride |
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| CN104671219A (en) * | 2013-12-02 | 2015-06-03 | 浙江化工院科技有限公司 | Sulfuric chloride separation and purification technique |
| CN106946231A (en) * | 2017-03-30 | 2017-07-14 | 杭州茂宇电子化学有限公司 | A kind of method and system for producing high-purity vikane |
| CN109369385A (en) * | 2018-11-12 | 2019-02-22 | 江山鑫隆化工有限公司 | A kind of preparation method of Trifluoroacetic Acid Ethyl Ester |
| CN109369385B (en) * | 2018-11-12 | 2021-06-04 | 江山鑫隆化工有限公司 | Preparation method of ethyl trifluoroacetate |
| CN115557471A (en) * | 2022-01-29 | 2023-01-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride and sulfuryl fluoride |
| CN114368728B (en) * | 2022-01-29 | 2022-11-08 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride |
| CN114368728A (en) * | 2022-01-29 | 2022-04-19 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride |
| WO2023142047A1 (en) * | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by electrofluorination |
| WO2023142027A1 (en) | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride |
| CN115557471B (en) * | 2022-01-29 | 2024-02-20 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride and sulfuryl fluoride |
| US12091315B2 (en) | 2022-01-29 | 2024-09-17 | Contemporary Amperex Technology Co., Limited | Method of preparing sulfuryl fluoride |
| CN116812876A (en) * | 2023-07-14 | 2023-09-29 | 河南省氟基新材料科技有限公司 | Preparation method of sulfuryl fluoride |
| CN116812876B (en) * | 2023-07-14 | 2024-08-09 | 河南省氟基新材料科技有限公司 | Preparation method of sulfuryl fluoride |
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