CN207294649U - A kind of device for preparing the misery thioesters of chloromethane - Google Patents

A kind of device for preparing the misery thioesters of chloromethane Download PDF

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Publication number
CN207294649U
CN207294649U CN201721320902.9U CN201721320902U CN207294649U CN 207294649 U CN207294649 U CN 207294649U CN 201721320902 U CN201721320902 U CN 201721320902U CN 207294649 U CN207294649 U CN 207294649U
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tank
tower
thioesters
misery
reactor
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杨振宁
周世刚
陈文志
张跃
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CHONGQING CHANGFENG CHEMICAL INDUSTRY Co Ltd
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CHONGQING CHANGFENG CHEMICAL INDUSTRY Co Ltd
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Abstract

Field of chemical equipment is the utility model is related to, specifically a kind of device for preparing the misery thioesters of chloromethane.Including reaction unit, extraction element, it is provided with nitrogen pot and the reaction unit is connected to by pipeline, and tail gas is set to destroy tower outside the reaction unit, the reaction unit is connected to the cleaning device by pipeline, the reaction unit includes solid phosgene tank, organic solution tank, tertiary amine catalyst tank, spicy thioalcohol tank, reactor, the cleaning device is connected to the extraction element by pipeline, the cleaning device includes pickling tower, caustic wash tower, salt water scrubber, the extraction element connects finished product kettle, the extraction element includes drier, it is evaporated under reduced pressure device.The utility model uses solid phosgene, and reaction condition is gentle, easy-to-operate, reduces the generation of accessory substance, improves product earning rate, tail gas is rationally handled, environmentally protective.

Description

A kind of device for preparing the misery thioesters of chloromethane
Technical field
Field of chemical equipment is the utility model is related to, specifically a kind of device for preparing the misery thioesters of chloromethane.
Background technology
Thio chloro-formate is a kind of important chemical products, is widely used in medicine, pesticide etc..Industrial production Thio chloro-formate, reacts generation at low temperature under catalyst using containing mercaptan with phosgene.Phosgene, also known as phosgene, High poison, non-ignitable, chemical reactivity is higher, meet water after have aggressive, be slightly soluble in water, be dissolved in aromatic hydrocarbons, benzene, carbon tetrachloride, The majority organic solvent such as chloroform, acetic acid, the industrial mixture using carbon monoxide and chlorine are made by activated carbon.Solid light Gas is called triphosgene, is a kind of widely used green chemical products, has in fine chemistry industry and organic synthesis field important Prospect, dissolves in the organic solvents such as dichloromethane, chloroform, ether, ethanol, tetrahydrofuran, toluene, it is opposite with for hypertoxic phosgene Boiling point is high, surface vapor pressure is low, heat endurance is high, is only handled as general poisonous substance, phosgene can be replaced to carry out a variety of organic anti- Should.
However, the one kind of the misery thioesters of chloromethane as thio chloro-carbonic acid, its Exploitation degree is far from enough, should give weight Depending on and develop, and other equipment for producing thio chloro-carbonic acids use gaseous state or liquid phosgene mostly, and reaction process is more fierce, Earning rate is not but high, and easily produces accessory substance, for this present situation, it is necessary to research and develop one kind prepare the misery thioesters of chloromethane can To do reactant using more stable, the safer solid phosgene of opposite gaseous state or liquid phosgene, and by-product produce are reduced as far as possible The raw device for improving product earning rate.
Utility model content
The utility model is in order to overcome above-mentioned technical problem, there is provided a kind of device for preparing the misery thioesters of chloromethane.
To achieve the above object, the utility model uses following technical scheme:
A kind of device for preparing the misery thioesters of chloromethane, including reaction unit, cleaning device, extraction element, are provided with nitrogen Tank is connected to the reaction unit by pipeline, and sets tail gas to destroy tower outside the reaction unit, and the reaction unit leads to Piping is connected to the cleaning device, and the cleaning device is connected to the extraction element, the extraction element by pipeline Connect finished product kettle.
Preferably, the reaction unit includes solid phosgene tank, organic solution tank, catalyst tank, spicy thioalcohol tank, reaction Device, the solid phosgene tank are connected to mixing tube with the organic solution tank, and solid phosgene is dissolved in organic in the mixing tube In solution, the mixing tube is connected to the reactor feed end, and the catalyst tank and the spicy thioalcohol tank directly pass through Pipeline is connected to the reactor feed end.
Preferably, being equipped with dropwise addition control valve with the mixing tube junction in the reactor, solution is slowly added dropwise To the inside reactor, reaction can be come into full contact with and can effectively control reaction process.
Preferably, it is equipped with agitating device in the reactor.
Preferably, the reactor adds the pungent of fixed amount every time using the operating type of intermittent addition reactant Mercaptan and phosgene solution, and the catalyst tank always conveys excess catalyst into the reactor in advance, reduces inessential The generation of chemical reaction, suppresses the generation of accessory substance.
Preferably, being equipped with temperature control equipment outside the reactor, the reaction temperature in the reactor can be controlled Degree and soaking time.
Preferably, the extraction element includes vacuumizing tower, filtration tank, described vacuumize in tower is equipped with aspiration pump, leads to Cross gas pipeline and connect the tail gas destruction tower, the tower discharge end that vacuumizes connects the filtration tank feed end, the filtering Tower discharge end connects the tail gas and destroys tower and the finished product kettle respectively again.
Preferably, the tail gas, which is destroyed in tower, is equipped with hydrolyst, while sequentially connected water is provided with outlet Absorb, alkali adsorption tower, tail gas destructive rate is up to more than 95%.
Beneficial effect is:A kind of device for preparing the misery thioesters of chloromethane of the utility model uses solid phosgene, reacts bar Part is gentle, easy-to-operate, more stablizes safety using the device of gaseous state or liquid phosgene than tradition, and passes through excessive Organic solvent and tertiary amine catalyst reduce the generation of accessory substance, improve product earning rate, tail gas are rationally handled, green ring Protect.
Brief description of the drawings
, below will be right in order to illustrate more clearly of the utility model embodiment or technical solution of the prior art Embodiment or attached drawing needed to be used in the description of the prior art are briefly described.In all of the figs, it is similar Element or part are generally identified by similar reference numeral.In attached drawing, each element or part might not be according to actual ratios Draw.
Fig. 1 is a kind of device flow chart for preparing the misery thioesters of chloromethane of the utility model.
Embodiment
The utility model is further described with reference to embodiment.
As shown in Figure 1, a kind of device for preparing the misery thioesters of chloromethane, including reaction unit, extraction element, it is provided with nitrogen Tank 6 is connected to the reaction unit by gas pipeline, is to the reaction unit after the completion of working as primary first-order equation using aspiration pump Excessive nitrogen is inside passed through, drives remaining phosgene and hydrogen chloride gas in reaction unit out of, and tail is set outside the reaction unit Gas destroys tower 7, and the remaining phosgene and hydrogen chloride gas in reaction unit enter tail gas by gas pipeline and destroy tower 7, the tail Gas destroys in tower 7 and is equipped with hydrolyst, and destroying the outlet of tower 7 in the tail gas is provided with sequentially connected water absorption, Alkali absorption Tower, tail gas destructive rate are environmentally protective up to more than 95%;The reaction unit is connected to the extraction element, institute by pipeline Stating reaction unit includes solid phosgene tank 1, organic solution tank 2, catalyst tank 3, spicy thioalcohol tank 4, reactor 5, the solid light Gas tank 1 is connected to mixing tube with the organic solution tank 2, and solid phosgene is substantially soluble in organic solution in mixing tube, described Mixing tube is connected to 5 feed end of reactor, and dropwise addition control is being equipped with the mixing tube junction in the reactor 5 Valve, phosgene solution are slowly added dropwise into inside the reactor 5, can be come into full contact with reaction and can effectively be controlled reaction process, light The usage amount of gas is relative to 1 mole of spicy thioalcohol, and usually more than 1 mole, be preferably 1.05~2 moles, 3 He of catalyst tank The spicy thioalcohol tank 4 is directly connected to 5 feed end of reactor by pipeline, and the reactor 5 uses intermittent addition The mode of reactant, catalyst and spicy thioalcohol are charged first in the reactor 5, and phosgene solution is slowly being dripped into reactor 5 Add, and the catalyst tank 3 always conveys excess tertiary amine catalyst into the reactor 5 in advance, and it is anti-to reduce inessential chemistry The generation answered, suppresses the generation of accessory substance, and reaction principle is as follows:
Agitating device is equipped with the reactor 5, it is ensured that two kinds of reactants can react completely in the reactor 5, The reactor 5 is externally provided with temperature control equipment, controls reaction temperature and soaking time in the reactor 5, described in holding Low-temperature condition is in reactor 5 under normal condition;The extraction element includes vacuumizing tower 8, filtration tank 9, described to vacuumize Is equipped with aspiration pump in tower 8, the solution in the reactor 5 after reaction be transported to described in vacuumize in tower 8, carry out vacuumizing place Reason, and be connected in described vacuumize in tower 8 equipped with gas passage in the tail gas destruction tower, the solution under vacuum state is defeated It is sent to be similarly in the filtration tank 9 of vacuum state and carries out filtration treatment, the finished product after extraction filtering is transported in finished product kettle 10, Solution after filtering, which is transported in liquid waste treating apparatus 11, carries out liquid waste processing.
Pass through above-described embodiment, it can be deduced that:A kind of device for preparing the misery thioesters of chloromethane of the utility model uses solid Phosgene, reaction condition is gentle, easy-to-operate, more stablizes safety using the device of gaseous state or liquid phosgene than tradition, and And the generation of accessory substance is reduced by excessive organic solvent and tertiary amine catalyst, and product earning rate is improved, it is reasonable to tail gas Processing, it is environmentally protective.
Although the foregoing describing specific embodiment of the present utility model, it will be appreciated by those of skill in the art that These are merely illustrative of, and the scope of protection of the utility model is defined by the appended claims.Those skilled in the art Member can make these embodiments numerous variations or repair on the premise of the principle and essence without departing substantially from the utility model Change, but these change and modification each fall within the scope of protection of the utility model.

Claims (8)

1. a kind of device for preparing the misery thioesters of chloromethane, including reaction unit, extraction element, it is characterised in that:It is provided with nitrogen Tank is connected to the reaction unit by gas pipeline, and sets tail gas to destroy tower, the reaction dress outside the reaction unit Put and the extraction element is connected to by pipeline, the extraction element is connected to the tail gas by gas pipeline and destroys tower, institute State extraction element discharge end and connect finished product kettle and liquid waste treating apparatus respectively again.
A kind of 2. device for preparing the misery thioesters of chloromethane according to claim 1, it is characterised in that:The reaction unit bag Include solid phosgene tank, organic solution tank, catalyst tank, spicy thioalcohol tank, reactor, the solid phosgene tank and the organic solution Tank is connected to mixing tube, and the mixing tube is connected to the reactor feed end, and the catalyst tank and the spicy thioalcohol tank are equal The reactor feed end is directly connected to by pipeline.
A kind of 3. device for preparing the misery thioesters of chloromethane according to claim 2, it is characterised in that:In the reactor It is equipped with the mixing tube junction and control valve is added dropwise.
A kind of 4. device for preparing the misery thioesters of chloromethane according to claim 2, it is characterised in that:Set in the reactor There is agitating device.
A kind of 5. device for preparing the misery thioesters of chloromethane according to claim 2, it is characterised in that:The reactor uses The intermittent operating type for adding reactant, adds the spicy thioalcohol and phosgene solution of fixed amount every time, and the catalyst tank is total It is to add excess tertiary amine catalyst into the reactor in advance.
A kind of 6. device for preparing the misery thioesters of chloromethane according to claim 2, it is characterised in that:Outside the reactor Equipped with temperature control equipment.
A kind of 7. device for preparing the misery thioesters of chloromethane according to claim 1, it is characterised in that:The extraction element bag Include and vacuumize tower, filtration tank, described vacuumize in tower is equipped with aspiration pump, and connecting the tail gas by gas pipeline destroys tower, institute State and vacuumize the tower discharge end connection filtration tank feed end, the filtration tank discharge end connects the tail gas and destroys tower respectively again With the finished product kettle.
A kind of 8. device for preparing the misery thioesters of chloromethane according to claim 1, it is characterised in that:The tail gas destroys tower It is interior to be equipped with hydrolyst, while sequentially connected water absorption, alkali adsorption tower are provided with outlet.
CN201721320902.9U 2017-10-13 2017-10-13 A kind of device for preparing the misery thioesters of chloromethane Active CN207294649U (en)

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CN201721320902.9U CN207294649U (en) 2017-10-13 2017-10-13 A kind of device for preparing the misery thioesters of chloromethane

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Application Number Priority Date Filing Date Title
CN201721320902.9U CN207294649U (en) 2017-10-13 2017-10-13 A kind of device for preparing the misery thioesters of chloromethane

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CN207294649U true CN207294649U (en) 2018-05-01

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