CN2354958Y

CN2354958Y - Apparatus for producing trichlorobenzylidyne

Info

Publication number: CN2354958Y
Application number: CN 97236927
Authority: CN
Inventors: 陈筱伯
Original assignee: Individual
Current assignee: Individual
Priority date: 1997-08-26
Filing date: 1997-08-26
Publication date: 1999-12-22
Anticipated expiration: 2007-08-26

Abstract

The utility model relates to an apparatus for producing benzenyl trichloride, which is composed of reaction kettles 1, 1', glass three-way pieces 15, 15', condensers 4, 4', condensers 5, 5', combined gas-phase liquid-phase separators 6, 6', liquid seal pipes 7, 7', spray heads 2, 2' and a plurality of sets of valves. Toluene which is arranged in the reaction kettles and chlorine gas is led into the reaction kettles are condensed for many times, and then the toluene and the chlorine gas which return to the reaction kettles are made into the benzenyl trichloride. The utility model has the advantages of lower raw material consumption of toluene and chlorine gas, higher quality for the by-product of hydrogen chloride, less environmental pollution, fewer chloride contained in the generated products, etc.

Description

The production equipment of benzotrichloride

The utility model relates to a kind of production equipment of benzotrichloride.

The normal method that adopts of main raw material benzotrichloride of producing Benzoyl chloride at present is that toluene makes through logical chlorine, and used initiator is the residual or dibenzoyl peroxide of ultraviolet, and this is reflected under 90 ℃～140 ℃ and carries out.In the production process of benzotrichloride, impurity such as chlorine, water, toluene, α-benzyl chloride, ω-dichloro methoxy, ω-trichlorotoluene zotrichloride, thiophene and 2-chlorothiophene can appear in the tail gas, under vacuum state, enter condenser with hydrogenchloride, wherein most of organism cooling back enters reactor by pipeline or liquid sealing pipe, chlorine residue and hydrogenchloride enter secondary reacting kettle, the wherein reaction of the toluene in chlorine residue and the secondary reacting kettle, hydrogenchloride enters the hydrochloric acid absorption unit at last.Chinese patent 96231483.8, a kind of " device of preparation benzotrichloride " disclosed, although this device can make toluene and chlorine consume hydrogenchloride low, that discharge and close characteristics such as impurity is low, but still has following defective: at first, still have a small amount of gas phase organism to take out of with hydrogenchloride; Secondly, logical chlorine structure of distributor in the reactor is undesirable, make the chlorine that feeds around the annular of container, not rise, but be monolateral rising, and make ascent direction vertical surface still wall liquid have the dead angle like this, have to not lead to chlorine by force when reaching standard to the later stage, cause chlorination on the ring of partial organic substances, distillation still residue increased after this was mainly reflected in synthetic Benzoyl chloride, and still closes muriate on a large amount of rings in residual, had increased environmental pollution.

The purpose of this utility model is will provide a kind of can make used raw material toluene and the production equipment of the benzotrichloride that chlorine consumption is lower, byproduct hydrogenchloride quality is higher, low in the pollution of the environment, the chloride in the product of generating obviously reduces.

The purpose of this utility model is achieved like this, a kind of production equipment of benzotrichloride, it comprises reactor 1,1 ', it is suitable for reading vertically to connect glass threeway 15 by pipeline respectively, 15 ', glass threeway 15,15 ' top connect condenser 4 by pipeline respectively, 4 ', at condenser 4,4 ' top connects another row condenser 5 by pipeline respectively, 5 ' top, condenser 5,5 ' the bottom connect built-up type gas phase liquid phase separator 6 by pipeline respectively, 6 ' top, built-up type gas phase liquid phase separator 6,6 ' the bottom respectively by liquid sealing pipe 7,7 ' through valve 9,9 ' with glass threeway 15,15 ' side valve connect, logical chlorine valve 11,11 ' respectively by pipeline and reactor 1, the shower nozzle 2 of 1 ' bottom, 2 ' connect, built-up type gas phase liquid phase separator 6,6 ' the tail gas mouth respectively by pipeline through valve 14,14 ' and valve 8 ', 8 backs and shower nozzle 2 ', 2 connect, the tail gas mouth simultaneously again respectively by pipeline through valve 13,13 ' back is connected with the hydrochloric acid absorption unit, dip tube 7,7 ' bottom connects valve 10 by pipeline respectively, 10 ', reactor 1,1 ' bottom connects valve 3,3 '.

Below in conjunction with accompanying drawing the utility model is further described below.

Fig. 1 is a structure principle chart of the present utility model.

Fig. 2 be

shower nozzle

2,2 of the present utility model ' structural representation.

Fig. 3 is the part sectioned view that revolves core 19 of the present utility model.

Fig. 4 is built-up type gas phase liquid phase separator 6 of the present utility model, 6 ' structural representation.

Shower nozzle

2,2 of the present utility model ' by inlet pipe 16, loam cake 17, trim ring 18, plug screw 27, revolve core 19, end cover 20 and form, inlet pipe 16 is fixed in the through hole 25 of loam cake 17, plug screw 27 is connected with the centre hole 28 that revolves core 19 by binding thread, revolve core 19, trim ring 18 and be located in revolving in the core chamber 31 of end cover 20 successively, loam cake 17 is connected by the top of binding thread and end cover 20, and with trim ring 18, revolve core 19 and compress.Offer some spiral slots 30 at the outer ledge that revolves core 19, centre hole 28 is opened in the centre of revolving core 19, and inclined hole 29 is opened in the cylindrical surface tangential direction of centre hole 28.Be provided with angle 26 in the bottom of trim ring 18, the effect of angle 26 is that the spiral slot 30 that prevents to revolve on the core 19 is covered by the end face of trim ring 18.When chlorine by through hole 25, the trim ring 18 of inlet pipe 16 through loam cake 17, because plug screw 27 is blocked the centre hole 28 that revolves core 19, so the spiral slot 30 that chlorine can only be through revolving core 19, inclined hole 29 and the curved tangential direction ejection from the bottom of revolving core chamber 31 and are upwards emitted after toluene in the reactor fully contacts again.Because the track of chlorine ejection is a spirrillum, thereby has increased the duration of contact of chlorine and toluene; Simultaneously, owing to chlorine sprays from revolving core arc tangential direction, thereby but the liquid in the driving a reaction still produces rotation, play stirring action, and make toluene and chlorine can fully obtain reacting.

Built-up type gas phase liquid phase separator 6,6 of the present utility model ' form by loam cake 21, container body 24, ripple porcelain plate 22, Glass tubing 23, loam cake 21 is connected with container body 24 by flange, ripple porcelain plate 22 has some, be installed in respectively in the container body 24, between every layer of ripple porcelain plate, be filled with the Raschig ring porcelain filling, have the hole, be inserted with Glass tubing 23 in it in the centre of ripple porcelain plate 22, center at loam cake 21 feeds vent line, and vent line communicates with Glass tubing 23.This device is attached on the ripple porcelain plate 22 after can making the gas phase organism condense into the liquid phase organism, rolls up drop and flows into liquid sealing pipe, thereby effectively suppressed the discharge of obnoxious flavour in the tail gas, has reduced atmospheric pollution.

Reactor 1 of the present utility model, 1 ' be F formula glassed steel reaction vessels, when this device work, if reactor 1 is the main reaction still, reactor 1 ' be secondary reacting kettle, at first shut-off valve 8,11 ', 13,10,10 ', 3,3 ', 14 ', 9,9 ' and glass threeway 15,15 ' side valve, open valve 11,14,8 ', 13 ' and glass threeway 15,15 ' on, following two valves, the toluene that measures is dropped into reactor 1 respectively, 1 ' in, and reactor heated, when being located at reactor 1,1 ' interior thermometer 12,12 ' on temperature when rising to 85 ℃, add an amount of initiator dibenzoyl peroxide again.Logical then chlorine, the inlet pipe 16 that chlorine enters shower nozzle 2 through valve 11, by the bottom ejection of shower nozzle 2 curved tangential directions from reactor 1, at this moment chlorine reacts with toluene on the one hand again; Feed liquid in driving a reaction still rotation on the other hand, and be the para-curve rising.After gas phase organism in the tail gas enters condenser 4, major part is got back in the reactor 1, remaining gas phase organism is after condenser 5 condensations, wherein most of gas phase organism is cooled to the liquid phase organism again and flows to built-up type gas phase liquid phase separator 6, and then store in the influent tube sealing 7, because of liquid sealing pipe 7 is that glass is made, wait to see that liquid phase organism in the liquid sealing pipe 7 are full after, open the side valve of valve 9 and glass threeway 15, make it to return in the reactor 1 automatically.And in the tail gas that is got off by condenser 5, behind the several layers ripple porcelain plate of a small amount of gas phase organism of institute's balance in built-up type gas phase liquid phase separator 6, repeated multiple times enlarges, dwindles, and the liquid that congeals into is attached on the ripple porcelain plate, rolls up drop and flows in the liquid sealing pipe 7.Tail gas hydrogenchloride passes through valve 14 with chlorine after built-up type gas phase liquid phase separator 6 separates, 8 ' enter the shower nozzle 2 of reactor 1 ' bottom ' in, by shower nozzle 2 ' curved tangential direction ejection, driving a reaction still 1 ' in liquid material rotation, and be para-curve and rise, this moment, chlorine reacted with reactor 1 ' interior excess toluene, the tail gas of reactor 1 ' generation is based on hydrogenchloride, it is with a small amount of gas phase organism through glass threeway 15 ' enter condenser 4 ' condensation, wherein most of gas phase organism be liquid phase and get back to reactor 1 ' in, surplus a small amount of organism with hydrogenchloride enter enter after condenser 5 ' condensation built-up type gas phase liquid phase separator 6 ', the liquid phase organism is in liquid sealing pipe 7 ' interior storage, after treating that liquid sealing pipe 7 ' interior is full, open valve 9 ' and glass threeway 15 ' side valve enter reactor 1 '.If after having less water to take condensation out of in reaction in toluene or the dibenzoyl peroxide, by built-up type gas phase liquid phase separator 6,6 ' enter liquid sealing pipe 7,7 ' bottom, finding after the water accumulation at any time can be by valve 10,10 ' emit.Gas phase organism in the tail gas then through built-up type gas phase liquid phase separator 6 ' after, the liquid phase of further congealing into organism and influent tube sealing 7 ', this moment tail gas in only remaining basically hydrogenchloride, it is by valve 13 ' enter hydrochloric acid absorption unit, because the hydrogenchloride of discharging is very clean, so synthetic hydrochloric acid quality is higher.The density of toluene reaches regulation density 1.396～1.398 o'clock in the question response still 1, and reaction finishes, and stops logical chlorine, cooling, and when treating to be designated as 50 ℃ on the thermometer 12, the bottom valve 3 of opening reactor 1 is standby with the product storage tank.Shut-off valve 3 again the toluene that measures is put into reactor 1,1 ', similar aforementioned process, with reactor 1 ' be the main reaction still, reactor 1 is a secondary reacting kettle, adjusts each valve, repeats aforesaid operations.

The utility model is because after adopting said structure, on the one hand, change the logical chlorine sparger in original reactor into shower nozzle, make chlorine and reaction of toluene more abundant, further reduced the consumption of toluene and chlorine, make simultaneously to contain ring in the benzotrichloride product of generation and go up muriate and obviously reduce, effectively choke suppress environmental pollution; On the other hand, behind the employing built-up type gas phase liquid phase separator, make the gas phase organism can be converted into the liquid phase organism effectively, reduced the discharge of obnoxious flavour, thereby guaranteed the quality of byproduct hydrogenchloride.

Claims

1, a kind of production equipment of benzotrichloride, it is characterized in that it comprises reactor (1), (1 '), it is suitable for reading vertically to connect glass threeway (15) by pipeline respectively, (15 '), glass threeway (15), the top of (15 ') connects condenser (4) by pipeline respectively, (4 '), in condenser (4), (4 ') top connects another row condenser (5) by pipeline respectively, the top of (5 '), condenser (5), the bottom of (5 ') connects built-up type gas phase liquid phase separator (6) by pipeline respectively, the top of (6 '), built-up type gas phase liquid phase separator (6), the bottom of (6 ') is respectively by liquid sealing pipe (7), (7 ') are through valve (9), (9 ') and glass threeway (15), the side valve of (15 ') connects, logical chlorine valve (11), (11 ') are respectively by pipeline and reactor (1), the shower nozzle (2) of (1 ') bottom, (2 ') connect, built-up type gas phase liquid phase separator (6), the tail gas mouth of (6 ') respectively by pipeline through valve (14), (14 ') and valve (8 '), (8) back and shower nozzle (2 '), (2) connect, the tail gas mouth simultaneously again respectively by pipeline through valve (13), (13 ') back is connected with the hydrochloric acid absorption unit, dip tube (7), (7 ') bottom connects valve (10) by pipeline respectively, (10 '), reactor (1), (1 ') bottom connects valve (3), (3 ').

2, the production equipment of benzotrichloride according to claim 1, it is characterized in that shower nozzle (2), (2 ') are by inlet pipe (16), loam cake (17), trim ring (18), plug screw (27), revolve core (19), end cover (20) is formed, inlet pipe (16) is fixed in the through hole (25) of loam cake (17), plug screw (27) is connected with the centre hole that revolves core (19) (28) by binding thread, revolve core (19), trim ring (18) is located in revolving in the core chamber (31) of end cover (20) successively, loam cake (17) is connected by the top of binding thread with end cover (20), and with trim ring (18), revolving core (19) compresses.

3, the production equipment of benzotrichloride according to claim 2, it is characterized in that offering some spiral slots (30) at the outer ledge that revolves core (19), centre hole (28) is opened in the centre of revolving core (19), and inclined hole (29) is opened in the cylindrical surface tangential direction of centre hole (28).

4, the production equipment of benzotrichloride according to claim 2 is characterized in that being provided with angle (26) in the bottom of trim ring (18).