CN113173831B - Production system and process for continuous chlorination of trichlorotoluene - Google Patents
Production system and process for continuous chlorination of trichlorotoluene Download PDFInfo
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- CN113173831B CN113173831B CN202110377325.1A CN202110377325A CN113173831B CN 113173831 B CN113173831 B CN 113173831B CN 202110377325 A CN202110377325 A CN 202110377325A CN 113173831 B CN113173831 B CN 113173831B
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- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 196
- XEMRAKSQROQPBR-UHFFFAOYSA-N (trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=CC=C1 XEMRAKSQROQPBR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 147
- 239000000463 material Substances 0.000 claims abstract description 50
- 238000010521 absorption reaction Methods 0.000 claims abstract description 44
- 238000007710 freezing Methods 0.000 claims abstract description 19
- 230000008014 freezing Effects 0.000 claims abstract description 19
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 239000012043 crude product Substances 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 239000000460 chlorine Substances 0.000 claims description 31
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 30
- 229910052801 chlorine Inorganic materials 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 21
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 18
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000012267 brine Substances 0.000 claims description 2
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract description 21
- 239000000047 product Substances 0.000 abstract description 5
- 239000012071 phase Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- CAHQGWAXKLQREW-UHFFFAOYSA-N Benzal chloride Chemical compound ClC(Cl)C1=CC=CC=C1 CAHQGWAXKLQREW-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000001000 anthraquinone dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012840 feeding operation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
- C07C17/14—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the side-chain of aromatic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production system and a production process for continuous chlorination of trichlorotoluene, wherein a toluene feeding pipe is arranged above a toluene metering tank, the toluene metering tank is communicated with a chlorination absorption kettle by a first pipeline, the chlorination absorption kettle is communicated with a first chlorination kettle by a first pressure pump through a pipeline, materials in the first chlorination kettle are sequentially communicated with a second chlorination kettle, a third chlorination kettle, a fourth chlorination kettle and a fifth chlorination kettle through overflow pipes, chlorine gas inlets are respectively arranged at the bottoms of the first chlorination kettle, the second chlorination kettle, the third chlorination kettle, the fourth chlorination kettle and the fifth chlorination kettle and are communicated with a chlorine gas inlet header pipe, gas outlets are respectively arranged at the tops of the first chlorination kettle, the second chlorination kettle, the third chlorination kettle, the fourth chlorination kettle and the fifth chlorination kettle and are respectively communicated with a chlorine gas discharge pipeline, and the chlorine gas discharge pipeline is sequentially communicated with a condenser and a freezing condenser. The invention is characterized by continuous feeding, continuous discharging, continuous chlorination, yield of chlorinated products of more than 98% and purity of crude products of more than 99%.
Description
Technical Field
The invention relates to the technical field of chemical technology, in particular to a production system and a process for continuous chlorination of trichlorotoluene.
Background
Trichlorotoluene, CAS number: 98-07-7, molecular formula: c (C) 7 H 5 Cl 3 Molecular weight: 195.474 it is used as basic raw material of dye, medical intermediate and ultraviolet absorber UV-9, UV-531, and organic synthesis intermediate to produce benzoic acid, benzoyl chloride, triphenylmethane dye, anthraquinone dye and quinoline dye. The traditional synthesis process is to put toluene into a chlorination kettle and heat the toluene to 90-120 DEGIntroducing chlorine gas, stopping chlorination reaction after the content of the dichlorotoluene is lower than 0.1%, and transferring the material into a rectifying still for rectifying to obtain the trichlorotoluene product. The intermittent reaction is adopted, the operation is complex, the working procedures are more, the energy consumption is high, and the productivity is low. The following problems are mainly present: firstly, the chlorine flow rate is low in the initial stage of the reaction, the material needs to be heated, the chlorine flow rate is large in the middle stage of the reaction, the reaction heat release amount is large, cooling is needed, the operation is complex, side reactions are more due to improper temperature control, and the impurity is large and the product quality is poor.
Disclosure of Invention
In order to solve the technical problems, the invention provides a production system and a production process for continuous chlorination of trichlorotoluene.
The technical scheme adopted by the invention is as follows:
the utility model provides a production system of trichlorotoluene continuous chlorination, including the toluene inlet pipe, toluene inlet pipe locates toluene metering tank top, toluene metering tank and chlorination absorption cauldron adopt first pipeline to communicate, chlorination absorption cauldron passes through the pipeline through first force pump and communicates with first chlorination cauldron, material in the first chlorination cauldron passes through overflow pipe and second chlorination cauldron, third chlorination cauldron, fourth chlorination cauldron and fifth chlorination cauldron communicate in proper order, first chlorination cauldron, second chlorination cauldron, third chlorination cauldron, fourth chlorination cauldron and fifth chlorination cauldron bottom are equipped with chlorine access and chlorine access house steward intercommunication respectively, first chlorination cauldron, second chlorination cauldron, third chlorination cauldron, fourth chlorination cauldron and fifth chlorination cauldron top are equipped with the gas discharge mouth respectively with chlorine exhaust pipeline intercommunication, chlorine exhaust pipeline communicates with condenser and cryocondenser in proper order, the bottom material discharge mouth of condenser communicates with first chlorination cauldron, the exhaust mouth of cryocondenser bottom, chlorination absorption cauldron top communicates with cryocondenser, the hydrogen chloride gas pipeline that is equipped with of cryocondenser is equipped with and is used for the hydrochloric acid absorption system to absorb hydrochloric acid to prepare.
Preferably, the upper part of the fifth chlorination reactor is provided with a crude product discharging pipeline.
Preferably, three condensers are arranged in series.
Preferably, a feed valve is arranged on the toluene feed pipe and is interlocked with the toluene storage tank liquid level.
Preferably, the toluene metering tank is arranged above the chlorination absorption kettle.
The production system is adopted to carry out the production process of the trichlorotoluene continuous chlorination, in the process, the temperature of the material in the chlorination absorption kettle is controlled by heating the material in the chlorination absorption kettle to 70-80 ℃ through steam, so that the residual chlorine can be reacted completely, and the reaction temperature of the material entering the chlorination kettle can be ensured.
Preferably, the temperature of the first chlorination reactor is controlled to be between 90 and 95 ℃, and the chlorine flow rate of the first chlorination reactor is not more than 110m 3 And/h, controlling the chlorine overflow amount.
Preferably, the temperature of the materials of the second chlorination reactor is controlled between 95 and 100 ℃, the temperature of the materials of the third chlorination reactor is controlled between 100 and 110 ℃, the temperature of the materials of the fourth chlorination reactor is controlled between 110 and 115 ℃, and the chlorine flow rates of the second chlorination reactor, the third chlorination reactor and the fourth chlorination reactor are respectively 140 to 160m 3 /h，170-190m 3 /h，230-250m 3 And/h, the chlorination reaction degree reaches 95%.
Preferably, the temperature of the material in the fifth chlorination reactor is controlled between 115 and 120 ℃, and the chlorine flow is controlled between 70 and 90m 3 And/h, ensuring the complete reaction of materials in the kettle and controlling the dichloro content below 0.05 percent.
Preferably, the gas phase condensed by the condenser is condensed again by the freezing condenser, the condenser is cooled by cooling water, the condensed material and residual chlorine enter the chlorination absorption kettle for reaction through a pipeline, all hydrogen chloride gas and the material are condensed again by the freezing condenser, the freezing condenser is cooled by freezing water, and the cryogenic condenser is condensed by cryogenic brine. The gas-phase and liquid-phase mixture materials cooled by the freezing condenser enter the absorption kettle for re-reaction, the gas-phase materials generated in the reaction process of the absorption kettle are condensed by the cryogenic condenser by using cryogenic salt water at the temperature of minus 20 ℃, organic components are thoroughly condensed into liquid phase and flow back to the absorption kettle, uncondensed hydrogen chloride gas is absorbed by water through a hydrogen chloride gas pipeline to prepare hydrochloric acid, and the content of organic matters in the hydrogen chloride is controlled to be the minimum.
Preferably, the first chlorination kettle, the second chlorination kettle, the third chlorination kettle and the fourth chlorination kettle and the fifth chlorination kettle are sequentially kept at a level difference of 95-105mm from high to low, so that smooth overflow of materials is ensured.
The invention has the beneficial effects that:
1. the invention is characterized by continuous feeding, continuous discharging, continuous chlorination, feeding control according to the liquid level of the discharged materials, yield of chlorinated products being more than 98% and crude product purity being more than 99%. The invention adopts continuous feeding, continuous discharging and continuous chlorination, the feeding is automatically supplemented according to the liquid level of the discharged material, the continuous feeding and the chlorination enable the temperature of each chlorination reaction kettle to be effectively controlled, and the reaction is stable. After the reaction is finished, the mixture is directly transferred into a rectifying still for rectification, so that the manual material transferring and feeding operation is omitted, and the labor is saved.
2. The 5 sets of chlorination kettles continuously react, the gas phases are communicated together to condense and recycle materials, the number of condensers is reduced, and multistage condensation is adopted, so that the materials are recycled more completely, and the equipment investment is reduced.
3. Each chlorination reaction kettle independently carries out chlorine gas introduction, each chlorination reaction kettle is provided with an independent chlorine gas introduction valve to control chlorine gas introduction flow according to set technological parameters, according to the difference of reaction stages, each kettle simultaneously introduces chlorine gas to improve the overall reaction speed, improve the production efficiency, the reaction is more stable and controllable, the chlorine gas introduction flow is controlled, the reaction is more stable, the control is convenient, and the chlorine gas reaction is more complete. The impurity generated by the reaction is less, and the product quality is high.
4. The chlorine flow of each chloridizing kettle can be stably controlled by the continuous chloridizing of the trichlorotoluene, the flow is not required to be regulated, the reaction is stable, the operation is simple and convenient, and the safety is higher.
Drawings
Fig. 1: the structure of the invention is schematically shown;
in the figure: the device comprises a toluene feeding pipe 1, a toluene metering tank 2, a chlorination absorption kettle 3, a first pipeline 4, a first pressure pump 5, a first chlorination kettle 6, an overflow pipe 7, a second chlorination kettle 8, a third chlorination kettle 9, a fourth chlorination kettle 10, a fifth chlorination kettle 11, a chlorine gas inlet main pipe 12, a chlorine gas outlet pipeline 13, a condenser 14, a freezing condenser 15, a cryogenic condenser 16, a hydrogen chloride gas pipeline 17 and a crude product discharging pipeline 18.
Detailed Description
Example 1
As shown in fig. 1, a production system for continuous chlorination of trichlorotoluene comprises a toluene feeding pipe 1, wherein the toluene feeding pipe 1 is arranged above a toluene metering tank 2, the toluene metering tank 2 is communicated with a chlorination absorption kettle 3 by adopting a first pipeline 4, the chlorination absorption kettle 3 is communicated with a first chlorination kettle 6 by adopting a pipeline through a first pressure pump 5, materials in the first chlorination kettle 6 are sequentially communicated with a second chlorination kettle 8, a third chlorination kettle 9, a fourth chlorination kettle 10 and a fifth chlorination kettle 11 through overflow pipes 7, chlorine gas inlets are respectively arranged at the bottoms of the first chlorination kettle 6, the second chlorination kettle 8, the fourth chlorination kettle 10 and the fifth chlorination kettle 11 and are communicated with a chlorine gas inlet manifold 12, gas outlets are respectively arranged at the tops of the first chlorination kettle 6, the second chlorination kettle 8, the third chlorination kettle 9, the fourth chlorination kettle 10 and the fifth chlorination kettle 11 and are respectively communicated with a chlorine gas outlet pipeline 13, the chlorine gas outlet pipeline 13 is sequentially communicated with a condenser 14 and a freezing condenser 15, the bottom material outlet of the condenser 14 is sequentially communicated with the first chlorination kettle 6, the bottom outlet of the condenser 15 is communicated with the chlorine gas outlet 3 is communicated with the absorption kettle 3, and the top of the cooling condenser 16 is communicated with the cooling absorption kettle 16 for preparing hydrochloric acid, and the deep-down system is used for preparing the hydrochloric acid is arranged at the top of the absorption kettle 16.
Preferably, a crude product discharging pipeline 18 is arranged at the upper part of the fifth chlorination kettle 11.
Preferably, three condensers 14 are provided in series.
Preferably, a feeding valve is arranged on the toluene feeding pipe 1 and is interlocked with the toluene storage tank liquid level. The feeding is automatically carried out according to the liquid level, the material liquid level in toluene and the resting time of toluene in the toluene metering tank 2 are ensured, the water and impurities in toluene can be completely precipitated to the bottom of the storage tank, and the separation is carried out periodically. And the toluene feeding pipe 1 is provided with a feeding valve which is interlocked with a toluene storage tank discharging valve and a toluene metering tank 2 liquid level. The feeding is automatically carried out according to the liquid level. The toluene storage tank is provided with a water dividing device, toluene entering the storage tank is kept stand for more than 2 hours, the water and impurities in the toluene can be guaranteed to be completely precipitated to the bottom of the storage tank, and the water is regularly separated, so that the water content of the toluene entering the toluene metering tank 2 is not more than 800ppm.
Preferably, the toluene metering tank 2 is arranged above the chlorination absorption kettle 3.
Preferably, the toluene metering tank 2 is arranged above the chlorination absorption kettle 3. The level difference is adopted for automatic feeding, the feeding valve of the first pipeline 4 is adopted for automatic feeding in a mode of interlocking with the liquid level of the chlorination absorption kettle 3, the feeding enters from the lower part, the discharging is discharged from the upper part, and the material residence time is ensured.
The production process for continuously chloridizing the trichlorotoluene by adopting the production system comprises the following steps of:
1. the hydrogen chloride gas generated in the chlorination process, residual chlorine and carried-out materials enter a condenser 14 through a gas phase pipe, the materials are cooled and enter a first chlorination kettle 6 through a recovery pipe, the uncondensed materials, unreacted chlorine and hydrogen chloride gas enter a freezing condenser 15 for cooling again, enter a chlorination absorption kettle 3 through a pipeline for recycling and reacting again, the unreacted chlorine completely reacts in the chlorination absorption kettle 3, the gas phase materials in the chlorination absorption kettle 3 react for cooling and refluxing again through a cryogenic condenser 16, and the hydrogen chloride gas enters a hydrochloric acid absorption system through a hydrogen chloride gas pipeline 17. The temperature of the first chlorination reactor 6 is controlled between 90 ℃ and 95 ℃, and the chlorine flow of the first chlorination reactor 6 is not more than 110m 3 And/h, controlling the chlorine overflow amount.
2. Chlorine enters each chlorination reactor through a chlorine inlet header 12 and a regulating valve.
Preferably, the toluene storage tank is higher than the chlorination absorption kettle 3 through the toluene feeding pipe 1, and the toluene automatically enters through the linkage of the feeding valve of the first pipeline 4 and the liquid level of the chlorination absorption kettle 3, and flows into the chlorination absorption kettle 3 through the level difference.
Preferably, the discharge port of the toluene metering tank 2 is arranged on the side surface of the storage tank, so that the water in the toluene is precipitated to the bottom of the storage tank, and the water diversion is performed periodically.
Preferably, the toluene inlet of the chlorination absorption kettle 3 is arranged at the lower part of the chlorination absorption kettle 3, the toluene feeding amount is controlled by interlocking the regulating valve with the liquid level of the chlorination absorption kettle 3, and the chlorination absorption kettle 3 controls the temperature so that the entered chlorine can completely react with toluene.
Preferably, the feed of the first chlorination reactor 6 enters through a pipeline 14, the feed is transferred into the first chlorination reactor through a first pressure pump 5, the feed control valve is adopted to carry out interlocking control adjustment with the liquid level of the first chlorination reactor 6, and the material enters from the lower part of the first chlorination reactor 6, and overflows to the next stage of chlorination reactor from the upper part.
Preferably, the first chlorination kettle 6, the second chlorination kettle 8, the third chlorination kettle 9, the fourth chlorination kettle 10 and the fifth chlorination kettle 11 are respectively communicated with each other through overflow pipes 7, all adopt upper and lower feeding, and the chlorinated materials are directly discharged into the next process through crude product discharging pipelines 18.
Preferably, the chlorine gas feed inlets of the first chlorination reactor 6, the second chlorination reactor 8, the third chlorination reactor 9, the fourth chlorination reactor 10 and the fifth chlorination reactor 11 are all arranged at the lower part, so that the chlorine gas is in contact with the materials for a long time, the reaction speed is improved.
Preferably, the gas-phase materials of the first chlorination kettle 6, the second chlorination kettle 8, the third chlorination kettle 9, the fourth chlorination kettle 10 and the fifth chlorination kettle 11 are communicated through a chlorine gas inlet main pipe 12, a three-stage cold condenser 14 is adopted for circulating water cooling, a freezing condenser 15 is adopted for freezing water cooling, a deep cooling water is adopted for the tail gas, a deep cooling water is adopted for cooling again by a deep cooling condenser 16, and the organic materials are completely condensed and recovered.
Preferably, the material temperature of the second chlorination kettle 8 is controlled to be 95-100 ℃, the material temperature of the third chlorination kettle 9 is controlled to be 100-110 ℃, the material temperature of the fourth chlorination kettle 10 is controlled to be 110-115 ℃, and the chlorine flow rates of the second chlorination kettle 8, the third chlorination kettle 9 and the fourth chlorination kettle 10 are respectively 150m 3 /h、180m 3 /h、240m 3 /h。
Preferably, the gas phase condensed by the condenser 14 is condensed again by the freezing condenser 15, the condenser 14 is cooled by cooling water, the gas phase and liquid phase mixture cooled by the freezing condenser 15 enters the absorption kettle 3 for re-reaction, all hydrogen chloride gas and materials are condensed again by the freezing condenser 15, the freezing condenser 15 is cooled by the freezing water, the gas phase materials generated in the reaction process of the absorption kettle 3 are condensed by the cryogenic condenser 16 by-20 ℃ of cryogenic saline water, the organic components are thoroughly condensed to be liquid phase and flow back to the absorption kettle 3, and the uncondensed hydrogen chloride gas is absorbed by water through the hydrogen chloride gas pipeline 17 to prepare hydrochloric acid. The organic matter content in the hydrogen chloride is controlled to be the minimum, and the hydrogen chloride gas is absorbed by water through a hydrogen chloride gas pipeline 17 to prepare hydrochloric acid.
Preferably, the first chlorination kettle 6, the second chlorination kettle 8, the third chlorination kettle 9 and the fourth chlorination kettle 10 and the fifth chlorination kettle 11 are sequentially arranged from high to low, and the potential difference of 100mm is kept, so that smooth overflow of materials is ensured.
Claims (6)
1. A process for the continuous chlorination of trichlorotoluene, the system employed in the process comprising a toluene feed pipe (1), characterized in that: the toluene feed pipe (1) is arranged above the toluene metering tank (2), the toluene metering tank (2) is communicated with the chlorination absorption kettle (3) by adopting a first pipeline (4), the chlorination absorption kettle (3) is communicated with the first chlorination kettle (6) through a first pressure pump (5), materials in the first chlorination kettle (6) are respectively communicated with the second chlorination kettle (8), the third chlorination kettle (9), the fourth chlorination kettle (10) and the fifth chlorination kettle (11) through overflow pipes (7), the first chlorination kettle (6), the second chlorination kettle (8), the third chlorination kettle (9), the fourth chlorination kettle (10) and the fifth chlorination kettle (11) are respectively provided with a chlorine inlet and a chlorine inlet header pipe (12), the tops of the first chlorination kettle (6), the second chlorination kettle (8), the third chlorination kettle (9), the fourth chlorination kettle (10) and the fifth chlorination kettle (11) are respectively provided with a gas exhaust pipeline (13), the chlorine exhaust pipeline (13) is respectively communicated with a condenser (14) and a condenser (15), the bottoms of the first chlorination kettle (14) and the condenser (15) are respectively communicated with a freezing material exhaust port (15), the top exhaust port of the chlorination absorption kettle (3) is communicated with a cryogenic condenser (16), and the cryogenic condenser (16) is provided with a hydrogen chloride gas pipeline (17) which is input into a hydrogen chloride absorption system for absorption so as to prepare hydrochloric acid;
in the process, the chlorination absorption kettle (3) is heated to 70-80 ℃ through steam, and the material temperature of the chlorination absorption kettle (3) is controlled, so that residual chlorine can be reacted completely, and the reaction temperature of the material entering the chlorination kettle can be ensured;
the condenser (14) is cooled by cooling water, the freezing condenser (15) is cooled by freezing water, and the cryogenic condenser (16) is condensed by cryogenic brine;
the temperature of the first chlorination reactor (6) is controlled to be 90-95 ℃, and the chlorine flow of the first chlorination reactor (6) is not more than 110m 3 Controlling the chlorine overflow amount; the material temperature of the second chlorination kettle (8) is controlled to be 95-100 ℃, the material temperature of the third chlorination kettle (9) is controlled to be 100-110 ℃, the material temperature of the fourth chlorination kettle (10) is controlled to be 110-115 ℃, and the chlorine introducing flow rates of the second chlorination kettle (8), the third chlorination kettle (9) and the fourth chlorination kettle (10) are respectively 140-160m 3 /h，170-190m 3 /h，230-250m 3 And/h, enabling the chlorination reaction degree to reach 95%;
the material temperature of the fifth chloridizing reactor (11) is controlled between 115 ℃ and 120 ℃ and the chlorine flow is 70 m to 90m 3 And/h, ensuring complete reaction of materials in the kettle, and controlling the dichloro content to be below 0.05%.
2. The production process for the continuous chlorination of trichlorotoluene according to claim 1, wherein: the upper part of the fifth chlorination reactor (11) is provided with a crude product discharging pipeline (18).
3. The production process for the continuous chlorination of trichlorotoluene according to claim 1, wherein: the condensers (14) are arranged in series.
4. The production process for the continuous chlorination of trichlorotoluene according to claim 1, wherein: and the toluene feeding pipe (1) is provided with a feeding valve which is interlocked with the liquid level of the toluene storage tank.
5. The production process for the continuous chlorination of trichlorotoluene according to claim 1, wherein: the toluene metering tank (2) is arranged above the chlorination absorption kettle (3).
6. The production process for the continuous chlorination of trichlorotoluene according to claim 1, wherein: the first chlorination kettle (6), the second chlorination kettle (8), the third chlorination kettle (9) and the fourth chlorination kettle (10) and the fifth chlorination kettle (11) are sequentially kept at a potential difference of 95-105mm from high to low.
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| CN113173831B true CN113173831B (en) | 2024-01-19 |
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| CN113173831A (en) | 2021-07-27 |
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Denomination of invention: A production system and process for continuous chlorination of trichlorotoluene Granted publication date: 20240119 Pledgee: Bank of China Limited by Share Ltd. Three Gorges Branch Pledgor: YIDU JOVIAN INDUSTRY CO.,LTD. Registration number: Y2024980026986 |