CN101250085B - Benzyl chloride continuous chlorination production technology - Google Patents

Benzyl chloride continuous chlorination production technology Download PDF

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Publication number
CN101250085B
CN101250085B CN200810014376A CN200810014376A CN101250085B CN 101250085 B CN101250085 B CN 101250085B CN 200810014376 A CN200810014376 A CN 200810014376A CN 200810014376 A CN200810014376 A CN 200810014376A CN 101250085 B CN101250085 B CN 101250085B
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chlorination
reactor
pipeline
benzyl chloride
benzyl
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Expired - Fee Related
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CN200810014376A
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CN101250085A (en
Inventor
董书国
李道杰
于佰胜
李银河
牛军
蔺清军
胡树国
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Shandong Liaocheng Zhongsheng Lanrui Chemical Industry Co., Ltd.
Liaocheng Luxi Chemical Engineering Co Ltd
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SHANDONG LIAOCHENG ZHONGSHENG LANRUI CHEMICAL INDUSTRY Co Ltd
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Abstract

The invention discloses a continuous chlorination method of benzyl chloride, which comprises a toluene tank connected with the upper of a chlorination column via a pipeline, wherein the top of the chlorination column is connected with a water condenser via a pipeline, the water condenser is connected with a salt water condenser, the water condenser and the salt water condenser are respectively connected with the pipeline, to feed reflux solution into the chlorination column, the bottom of the chlorination column via a first gas exit tube is connected with a first reaction vessel and via a second gas exit tube is connected with a second reaction vessel, the bottom of the first reaction vessel via a crude benzyl pipe is connected with the bottom of the second reaction vessel, and the bottomof the second reaction vessel is connected with a crude benzyl middle ladel via a crude benzyl pipe. The continuous chlorination method has the advantages that the invention completely changes the chlorination discontinuous production of benzyl chloride, to improve production efficiency significantly and can continuously produce without stop for cleaning materials, thereby improving 25% of effective yield. The benzyl chloride content of the product can reach 95%.

Description

The benzyl chloride continuous chlorination production technology device
Technical field
The present invention relates to the production technique of Benzyl Chloride, a kind of benzyl chloride continuous chlorination production technology device of accurately saying so.
Background technology
Benzyl Chloride is a kind of important organic intermediate, and industrial goods are colourless or light yellow transparent liquid, and irritating smell is arranged, and corrodibility is stronger, can be dissolved in organic solvents such as ether, chloroform, chlorobenzene.Benzyl Chloride is industrial of many uses, be mainly used in agricultural chemicals, medicine, spices, colour additive, additive synthesis field, in order to products such as Development and Production phenyl aldehyde, butyl benzyl phthalate, aniline, Volaton, benzylpenicillin, phenylcarbinol, benzyl cyanide, toluylic acids.
At present, domestic Benzyl Chloride chlorination production technology all adopts the batch production mode, that is: from reactor bottom charging, bottom discharge, the reactor that uses is an enamel still, the deficiency of this production technique is: owing to be batch production, enamel reaction still is subjected to the temperature difference influence of material bigger, makes the temperature variation of reactor bigger, has a strong impact on the work-ing life of reactor under big temperature head; Owing to be batch production, be example with every reaction 8500L Benzyl Chloride, its reaction times needs about 30 hours, and the cleaning material that needs simultaneously to stop is restarted again, makes production efficiency lower; The while plant factor is lower etc.
Summary of the invention
The purpose of this invention is to provide a kind of benzyl chloride continuous chlorination production technology device, it improves at the deficiency of existing technology, changes batch production into continuous chlorination production, thereby reaches the purpose of enhancing productivity.
The present invention for achieving the above object, be achieved through the following technical solutions: the benzyl chloride continuous chlorination production technology device, comprise the toluene jar, the toluene jar is connected with chlorination tower top by first pipeline, the chlorination top of tower is connected with water condenser by second pipeline, water condenser is connected with brine condenser, water condenser and brine condenser respectively with first pipe connection, phegma is entered in the chlorination tower, first pipeline, one end is connected with the toluene jar, the other end is connected with chlorination tower top, the chlorination tower bottom is connected with first reactor by first riser, the chlorination tower bottom is connected with second reactor by second riser, and first reactor bottom is connected with second reactor bottom by thick benzyl flow duct, and second reactor bottom is connected with thick benzyl tundish by thick benzyl pipeline.Water condenser and brine condenser are interconnected at the top, and water condenser is water, top circulating backwater on bottom cycle, brine condenser in the bottom freezing on water, the freezing backwater in top.Temperature of charge in first reactor and second reactor is respectively 150 ℃-190 ℃.Baffle plate is installed in second riser, and the area of baffle plate is the second riser circumference volumetrical 1/5th to 1/3rd, leaves cavity between the baffle plate upper end and second riser, and this cavity communicates with second riser.In first pipeline liquid flow rate be the 100-300 liter/hour.
Positively effect of the present invention is: it has thoroughly changed the chlorination batch production technology of Benzyl Chloride, makes production efficiency obtain bigger raising, and it can continuously be produced, the cleaning material that do not need to stop, and useful output has improved about 25%; Owing to be continuous production processes, make the temperature of reactor keep constant temperature substantially, and influence when little, thereby can increase substantially work-ing life of reactor, and reduced production cost when enamel reaction still is subjected to temperature of charge; Owing to adopt the mode of chlorination top of tower charging, can reduce energy expenditure etc. effectively to system's cooling; Benzyl Chloride content with explained hereafter of the present invention can reach about 95%.
Description of drawings
Accompanying drawing 1 is a technological process of production sketch of the present invention; Accompanying drawing 2 is I portion structure for amplifying synoptic diagram in second riser in the accompanying drawing 1; Accompanying drawing 3 be in the accompanying drawing 1 in second riser A-A analyse and observe the structure for amplifying synoptic diagram.
Embodiment
Production technique of the present invention is to adopt the production technique device of continuous chlorination in the production process of Benzyl Chloride, except that normal maintenance, does not need to stop.Various device that uses in the production technique and technology are: toluene jar 1 is set, toluene in the toluene jar 1 is imported by the toluene pump, toluene jar 1 is connected with chlorination tower 3 tops by first pipeline 2, chlorination tower 3 tops are connected with water condenser 15 by second pipeline 11, water condenser 15 is connected with brine condenser 14, water condenser 15 is connected with first pipeline 2 respectively with brine condenser 14, phegma is entered in the chlorination tower 3, first pipeline, 2 one ends are connected with toluene jar 1, the other end is connected with chlorination tower 3 tops, chlorination tower 3 bottoms are connected with first reactor 5 by first riser 4, chlorination tower 3 bottoms are connected with second reactor 8 by second riser 9, first reactor, 5 bottoms are connected with second reactor, 8 bottoms by thick benzyl flow duct 6, and second reactor, 8 bottoms are connected with thick benzyl tundish 7 by thick benzyl pipeline 13.Water condenser 15 and brine condenser 14 are interconnected at the top, and water condenser 15 is water, top circulating backwater on bottom cycle, brine condenser 14 in the bottom freezing on water, the freezing backwater in top.Temperature of charge in first reactor 5 and second reactor 8 is respectively 150 ℃-190 ℃.In second riser 9 baffle plate 10 is installed, the area of baffle plate 10 is second riser, 9 circumference volumetrical 1/5th to 1/3rd, leaves cavity between baffle plate 10 upper ends and second riser 9, and this cavity communicates with second riser 9.In first pipeline 2 liquid flow rate be the 100-300 liter/hour.
Concrete production technique is: the preparation work before driving is: toluene is inserted respectively in first reactor 5 and second reactor 8, and the amount of inserting is 8500L, and equivalent is distributed in two reactors, and the capacity in this reactor can be determined according to production technique ability size.Toluene is inserted in the toluene jar 1, to first reactor 5 and 8 heating of second reactor, reactor adopts enamel to make, use heat-conducting oil heating, Heating temperature slowly rises, slowly be warming up to 150-190 ℃, treat on the column plate of chlorination tower 3 thing liquid measure logical chlorine in chlorination tower 3 just often, logical amount of chlorine be the 10-30 cubic meter/hour until reach positive normal open amount of chlorine be the 50-100 cubic meter/hour.
After the driving toluene is continuously inserted in the toluene jar 1, toluene is flowed into by chlorination tower 3 tops by first pipeline 2, simultaneously, the mixed gas of hydrogenchloride and toluene enters in the water condenser 15 by chlorination tower 3 tops second pipeline 11, to be back to after the toluene condensation in first pipeline 2, because water condenser 15 is connected by pipeline 12 with brine condenser 14, so, the mixed gas of hydrogenchloride and toluene in brine condenser 14 further with the toluene condensation, it is back in first pipeline 2, and hydrogenchloride enters retrieving arrangement by the tail gas extraction duct.The flow of toluene in first pipeline 2 be the 100-300 liter/hour, this can keep reacting preferably, and make productive rate remain on better level, the flow that need keep when this flow is ordinary production, that is: be the flow that toluene jar 1 is imported in chlorination tower 3, do not comprise water condenser 15 and brine condenser 14 quantity of reflux.Chlorination tower 3 is worked under the illumination state, liquid in the chlorination tower 3 enters in first reactor 5 by first riser 4, liquid in the chlorination this moment tower 3 is the mixture of Benzyl Chloride and toluene, flow in second reactor 8 by Benzyl Chloride pipeline 6 through reacted Benzyl Chloride crude product in first reactor 5, and then enter in the thick benzyl tundish 7 by thick benzyl pipeline 13.Owing in second riser 9 baffle plate 10 is installed, baffle plate 10 is with a part of cavity shutoff in second riser 9, the volume of blocking pipe circumferential direction is 1/5th to 1/3rd, to guarantee that liquid can not flow in second reactor 8, simultaneously, in the smooth and easy backflow chlorination tower 3 of gas energy in second reactor 8.Because the liquid in the chlorination tower 3 can not flow in second reactor 8, so material flows in second reactor 8 in first reactor 5, the Benzyl Chloride crude product can only flow out in second reactor 8, can obtain the higher Benzyl Chloride of content.Gas in first riser 4 is back in the chlorination tower 3 equally.The Benzyl Chloride crude product obtains the Benzyl Chloride product by rectification under vacuum after entering thick benzyl tundish 7 again.Described rectification under vacuum method adopts known technology to finish.
Technology of the present invention not detailed description is known technology.

Claims (5)

1. benzyl chloride continuous chlorination production technology device, comprise toluene jar (1), it is characterized in that: toluene jar (1) is connected with chlorination tower (3) top by first pipeline (2), chlorination tower (3) top is connected with water condenser (15) by second pipeline (11), water condenser (15) is connected with brine condenser (14), water condenser (15) is connected with first pipeline (2) respectively with brine condenser (14), phegma is entered in the chlorination tower (3), first pipeline (2) one ends are connected with toluene jar (1), the other end is connected with chlorination tower (3) top, chlorination tower (3) bottom is connected with first reactor (5) by first riser (4), chlorination tower (3) bottom is connected with second reactor (8) by second riser (9), first reactor (5) bottom is connected with second reactor (8) bottom by thick benzyl flow duct (6), and second reactor (8) bottom is connected with thick benzyl tundish (7) by thick benzyl pipeline (13).
2. benzyl chloride continuous chlorination production technology device according to claim 1, it is characterized in that: water condenser (15) is interconnected at the top with brine condenser (14), water condenser (15) is water, top circulating backwater on bottom cycle, brine condenser (14) in the bottom freezing on water, the freezing backwater in top.
3. benzyl chloride continuous chlorination production technology device according to claim 1 is characterized in that: the temperature of charge in first reactor (5) and second reactor (8) is respectively 150 ℃-190 ℃.
4. benzyl chloride continuous chlorination production technology device according to claim 1, it is characterized in that: baffle plate (10) is installed in second riser (9), the area of baffle plate (10) is second riser (a 9) circumference volumetrical 1/5th to 1/3rd, leave cavity between baffle plate (10) upper end and second riser (9), this cavity communicates with second riser (9).
5. benzyl chloride continuous chlorination production technology device according to claim 1 is characterized in that: in first pipeline (2) liquid flow rate be the 100-300 liter/hour.
CN200810014376A 2008-03-13 2008-03-13 Benzyl chloride continuous chlorination production technology Expired - Fee Related CN101250085B (en)

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CN101250085B true CN101250085B (en) 2010-05-26

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CN113072418A (en) * 2021-03-04 2021-07-06 老河口华辰化学有限公司 Production method for double-kettle switching continuous chlorination

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2859253A (en) * 1955-10-19 1958-11-04 Heyden Newport Chemical Corp Process for the continuous preparation of benzyl chloride
CN1982266A (en) * 2005-12-13 2007-06-20 张国胜 Method for continuouslly dewatering toluene during process of benzyl chloride
CN101070265A (en) * 2007-06-18 2007-11-14 南京工业大学 Method for producing benzyl chloride compound
CN201003039Y (en) * 2007-02-10 2008-01-09 张国胜 Apparatus for producing benzyl chloride

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2859253A (en) * 1955-10-19 1958-11-04 Heyden Newport Chemical Corp Process for the continuous preparation of benzyl chloride
CN1982266A (en) * 2005-12-13 2007-06-20 张国胜 Method for continuouslly dewatering toluene during process of benzyl chloride
CN201003039Y (en) * 2007-02-10 2008-01-09 张国胜 Apparatus for producing benzyl chloride
CN101070265A (en) * 2007-06-18 2007-11-14 南京工业大学 Method for producing benzyl chloride compound

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Inventor after: Zhang Jincheng

Inventor after: Dong Shuguo

Inventor after: Li Daojie

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Inventor after: Niu Jun

Inventor after: Lin Qingjun

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