WO2015032213A1 - Chlorine introducing method for 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method - Google Patents
Chlorine introducing method for 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method Download PDFInfo
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- WO2015032213A1 WO2015032213A1 PCT/CN2014/077655 CN2014077655W WO2015032213A1 WO 2015032213 A1 WO2015032213 A1 WO 2015032213A1 CN 2014077655 W CN2014077655 W CN 2014077655W WO 2015032213 A1 WO2015032213 A1 WO 2015032213A1
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- Prior art keywords
- chlorine
- chlorination
- tank
- kettle
- valve
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000000460 chlorine Substances 0.000 title claims abstract description 117
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 23
- ITNMAZSPBLRJLU-UHFFFAOYSA-N 2,6-dichloro-4-(trifluoromethyl)aniline Chemical compound NC1=C(Cl)C=C(C(F)(F)F)C=C1Cl ITNMAZSPBLRJLU-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 107
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 10
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- ODGIMMLDVSWADK-UHFFFAOYSA-N 4-trifluoromethylaniline Chemical compound NC1=CC=C(C(F)(F)F)C=C1 ODGIMMLDVSWADK-UHFFFAOYSA-N 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- 229910002804 graphite Inorganic materials 0.000 claims description 28
- 239000010439 graphite Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 13
- 150000001412 amines Chemical class 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- WGTOHHOXVMDCHD-UHFFFAOYSA-N 4-(trifluoromethyl)aniline Chemical compound FC(C1=CC=C(N)C=C1)(F)F.FC(C1=CC=C(N)C=C1)(F)F WGTOHHOXVMDCHD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008346 aqueous phase Substances 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 5
- 239000011265 semifinished product Substances 0.000 claims description 4
- 239000006200 vaporizer Substances 0.000 claims 4
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005070 sampling Methods 0.000 abstract description 2
- 230000000712 assembly Effects 0.000 abstract 2
- 238000000429 assembly Methods 0.000 abstract 2
- 238000010025 steaming Methods 0.000 abstract 1
- JXTHNDFMNIQAHM-UHFFFAOYSA-N dichloroacetic acid Chemical compound OC(=O)C(Cl)Cl JXTHNDFMNIQAHM-UHFFFAOYSA-N 0.000 description 24
- BHAOWKAHKDUCLU-UHFFFAOYSA-N ClC1=C(N)C(=CC(=C1)C(F)(F)F)Cl.Cl Chemical compound ClC1=C(N)C(=CC(=C1)C(F)(F)F)Cl.Cl BHAOWKAHKDUCLU-UHFFFAOYSA-N 0.000 description 13
- 229960005215 dichloroacetic acid Drugs 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- CSVFWMMPUJDVKH-UHFFFAOYSA-N 1,1-dichloropropan-2-one Chemical compound CC(=O)C(Cl)Cl CSVFWMMPUJDVKH-UHFFFAOYSA-N 0.000 description 6
- IZRMJONVEVZERC-UHFFFAOYSA-N 2,2-dichloroethanimidamide Chemical compound NC(=N)C(Cl)Cl IZRMJONVEVZERC-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 238000004807 desolvation Methods 0.000 description 2
- 229940120124 dichloroacetate Drugs 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- VXIVSQZSERGHQP-UHFFFAOYSA-N chloroacetamide Chemical compound NC(=O)CCl VXIVSQZSERGHQP-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- -1 dichloroacetyl Chemical group 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C209/74—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton by halogenation, hydrohalogenation, dehalogenation, or dehydrohalogenation
Definitions
- the present invention relates to a 3,5-dichloro-4-aminobenzotrifluoride chloride process, and to a chlorine system for use in a 3,5-dichloro-4-aminobenzotrifluoride chloride process.
- the liquid chlorination reaction is that the liquid chlorine is heated and vaporized and then introduced into the material from the upper part of the reactor. Due to the internal stirring of the reactor or other reasons, the depth of the chlorine tube inserted into the kettle is limited, so there is always a comparison.
- the chlorine gas is too late to react and volatilizes and enters the tail gas absorption system together with the hydrogen chloride gas. Due to the presence of more chlorine gas, not only the raw material liquid chlorine is wasted, but also the burden of the exhaust gas absorption system is increased, and the alkali used for exhaust gas absorption is greatly increased. Liquid, which increases the cost of the company's products. Not only does it cause a lot of pollution to the environment, but it also wastes a large part of the resources (liquid chlorine), which costs money and pollutes the environment.
- the present invention provides a 3,5-dichloro-4-aminobenzotrifluoride chloride process, and a chlorine system for use in a 3,5-dichloro-4-aminobenzotrifluoride chloride process.
- the 3, 5-dichloro-4-aminobenzotrifluoride chloride method comprises the following steps:
- a chlorine-passing system in a 3,5-dichloro-4-aminotrifluorotoluene chloride process comprising a plurality of sets of chlorination equipment components
- the chlorination plant component comprising a chlorination kettle, a chlorine buffer tank a chlorine gas cylinder and a gasifier, wherein the top of the chlorination kettle is respectively connected with a graphite condenser, a high-level tank for a chlorine metering tank of an amine metering tank, a buffer tank for chlorine gas, and a graphite heat exchange between the chlorination tank and the graphite condenser.
- a chlorine valve in the chlorine passage between the chlorination tank and the chlorine buffer tank is arranged near the chlorination kettle end, and a chlorine inlet valve is arranged on the chlorine passage between the chlorination kettle and the chlorine buffer tank.
- a chlorine gas buffer tank end is provided with a pipeline cut-off valve, and the chlorine pipeline is further provided with a flow inlet and outlet wide door, and a feed valve is arranged between the chlorine gas inlet and the cut-off valve of the chlorination kettle, and the chlorine connecting gas is arranged a gasifier connected to the chlorine gas bottle and the hot water tank, wherein the gasifier and the chlorine gas bottle are provided with a chlorine tube needle circle, and the bottom of the chlorination kettle is connected with the chlorination intermediate tank and the settling tank, Connecting the solvent tank at the bottom of the chlorination intermediate tank and desolving the solvent tank connection Chloroacetamide embankment receiving groove, the receiving groove dichloroacetyl embankment graphite condenser connected to the desolvation tank connected caus
- the chlorine at the bottom greatly saves the amount of liquid chlorine, which saves the original
- the material has reduced the liquid alkali used for exhaust gas absorption, and has achieved considerable economic benefits. At the same time, it has reduced environmental pollution and achieved good environmental benefits.
- Figure 1 is a schematic view of the structure of the present invention.
- the 3,5-dichloro-4-aminobenzotrifluoride chloride method of the present invention comprises the following steps:
- a chlorine-passing system in a 3, 5-dichloro-4-aminobenzotrifluoride chloride process comprising two sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle 1, a chlorine buffer tank 2.
- a chlorine gas bottle 3 and a gasifier 4 wherein the top of the chlorination kettle 1 is connected to a graphite condenser 5, an amine metering tank 6, a dichloroacetic acid high level tank 7, a chlorine gas buffer tank 2, and the chlorination tank 1 and A graphite heat exchanger valve 8 is disposed between the graphite condenser 5, and a chlorination kettle chlorine gas valve 9 is disposed on the chlorine passage 22 between the chlorination kettle 1 and the chlorine buffer tank 2 near the chlorination tank 1 end.
- a chlorine outlet pipe 22 between the chlorination tank 1 and the chlorine buffer tank 2 is provided with a pipe shut-off valve 10 near the chlorine buffer tank 2, and the flow passage 22 is further provided with a flow inlet and outlet port 23,
- a feed valve 11 is disposed between the chlorination kettle chlorine gas 9 and the pipeline shutoff valve 10, and the chlorine buffer tank 2 is connected to the gasifier 4, and the gasifier 4 is connected to the chlorine gas cylinder 3 and the hot water tank 12,
- a gas chloride needle valve 13 is disposed between the gasifier 4 and the chlorine gas bottle 3, and the bottom of the chlorination kettle 1 is connected to the chlorination.
- the tank 14 and the settling tank 15, the bottom of the chlorination intermediate tank 14 is connected with a solvent tank 16 and a desolvent tank 17, and the solvent tank 16 is connected to the dichloroacetone receiving tank 18, and the dichloroacetone receiving tank 18 is connected to the graphite.
- the condenser 19 is connected to the alkali washing tank 20, and a semi-finished pump 21 is disposed between the alkali washing tank 20 and the desolvent tank 17.
- Example 2 As shown in Fig. 1, the 3,5-dichloro-4-aminobenzotrifluoride chloride method of the present invention comprises the following steps:
- a chlorine-passing system in a 3, 5-dichloro-4-aminobenzotrifluoride chloride process comprising two sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle 1, a chlorine buffer tank 2.
- a chlorine gas bottle 3 and a gasifier 4 wherein the top of the chlorination kettle 1 is connected to a graphite condenser 5, an amine metering tank 6, a dichloroacetic acid high level tank 7, a chlorine gas buffer tank 2, and the chlorination tank 1 and Between the graphite condenser 5 a graphite heat exchanger valve 8, a chlorine gas pipe 22 between the chlorination kettle 1 and the chlorine buffer tank 2 is disposed near the chlorination tank 1 and is provided with a chlorination kettle into the chlorine gas 9, the chlorination kettle 1 and chlorine gas A chlorine shut-off valve 10 is disposed on the chlorine-passing pipe 22 between the buffer tanks 2 near the chlorine buffer tank 2, and a flow-in and out-out valve 23 is further disposed on the chlorine-passing pipe 22, and the chlorination kettle enters the chlorine gas pottery 9 A feed valve 11 is disposed between the line shutoff valve 10 and the chlorine buffer tank 2 is connected to the gasifier 4, and the gasifier 4 is connected to a chlorine gas bottle 3 and a
- a chlorine tube needle valve 13 is disposed between the bottles 3, and the bottom of the chlorination tank 1 is connected with a chlorination intermediate tank 14 and a settling tank 15, and the bottom of the chlorination intermediate tank 14 is connected with a solvent tank 16 and a desolvent tank 17,
- the solvent tank 16 is connected to the dichloroacetone receiving tank 18, and the dichloroacetone receiving tank 18 is connected to the graphite condenser 19, and the desolvent tank 17 is connected to the alkali washing tank 20, the alkali washing tank 20 and the desolvent kettle.
- a semi-finished product pump 21 is provided between the 17th.
- the 3,5-dichloro-4-aminobenzotrifluoride chloride method of the present invention comprises the following steps:
- the intermediate layer collects the chlorination to be batched to obtain 3,5-dichloro-4-aminobenzotrifluoride, and the aqueous phase is discharged into the settling tank 15.
- a chlorine-passing system in a 3, 5-dichloro-4-aminobenzotrifluoride chloride process comprising two sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle 1, a chlorine buffer tank 2.
- a chlorine gas bottle 3 and a gasifier 4 wherein the top of the chlorination kettle 1 is connected to a graphite condenser 5, an amine metering tank 6, a dichloroacetic acid high level tank 7, a chlorine gas buffer tank 2, and the chlorination tank 1 and A graphite heat exchanger valve 8 is disposed between the graphite condensers 5, and a chlorination tank is provided with a chlorine gas 9 on the chlorine passage 22 between the chlorination tank 1 and the chlorine buffer tank 2, near the chlorination tank 1 end.
- a chlorine shut-off valve 10 is disposed on the chlorine-passing pipe 22 between the chlorination tank 1 and the chlorine buffer tank 2 near the chlorine buffer tank 2, and the gas-passing pipe 22 is further provided with a flow inlet and outlet door 23,
- a feed valve 11 is disposed between the chlorination kettle and the gas shutoff valve 10, and the chlorine buffer tank 2 is connected to the gasifier 4, and the gasifier 4 is connected to the chlorine gas bottle 3 and the hot water tank 12,
- a gas chloride needle valve 13 is disposed between the gasifier 4 and the chlorine gas cylinder 3, and the bottom of the chlorination kettle 1 is connected to the middle of the chlorination.
- the desolvent tank 17 is connected to the alkali washing tank 20, and a semi-finished product pump 21 is disposed between the alkali washing tank 20 and the desolvent tank 17.
- the chlorine at the bottom greatly saves the amount of liquid chlorine, which not only saves raw materials, but also reduces the liquid alkali used for exhaust gas absorption, and has achieved considerable economic benefits. At the same time, it has reduced environmental pollution and achieved good environmental benefits.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Disclosed are a chlorine introducing method for 3,5-dichloro-4-aminotrifluorotoluene and a chlorine introducing system applied to the chlorine introducing method. The chlorine introducing method for 3,5-dichloro-4-aminotrifluorotoluene comprises the following steps: checking each piece of equipment of the chlorine introducing system; feeding 4-amino-trifluorotoluene into a chlorination kettle; placing dichloroethane into the chlorination kettle; adding water; steaming; starting chlorination; introducing liquid chlorine into a hot water tank; sampling and analyzing; and after the chlorine introduction is finished, layering. The chlorine introducing system comprises two sets of chlorination equipment assemblies, and the chlorination equipment assemblies comprise the chlorination kettle 1, a chlorine buffer tank 2, a chlorine cylinder 3 and a gasifier 4. The present invention has the following beneficial effects: chlorine is introduced from the bottom, so the amount of the liquid chlorine used is greatly reduced, raw materials are saved, liquid alkali used for tail gas absorption is reduced, a considerable economic benefit is obtained, and at the same time the environmental pollution is reduced and a better environmental benefit is achieved.
Description
3， 5-二氯- 4-氨基三氟甲苯通氯方法及其应用于该通氯方法中的通氯系统 技术领域 3, 5-dichloro-4-aminobenzotrifluoride chloride method and chlorine application system thereof in the chlorine method
本发明涉及一种 3， 5-二氯 -4-氨基三氟甲苯通氯方法， 还涉及一种应 用于 3， 5-二氯 -4-氨基三氟甲苯通氯方法中的通氯系统。 The present invention relates to a 3,5-dichloro-4-aminobenzotrifluoride chloride process, and to a chlorine system for use in a 3,5-dichloro-4-aminobenzotrifluoride chloride process.
背景技术 Background technique
长期以来， 液氯氯化的反应都是液氯经加热汽化后从反应釜上部通入 物料中， 由于反应釜内部搅拌或其他原因， 限制了通氯管插入釜内的深度， 所以总有较多的氯气来不及反应而挥发出来和氯化氢气体一并进入尾气吸 收系统， 由于存在较多的氯气， 不仅浪费了原料液氯， 增加了尾气吸收系 统的负担， 同时也大大增加了尾气吸收所用的碱液， 增加了企业的产品成 本。 不仅对环境造成了较大污染， 又浪费了很大一部分资源 （液氯）， 既浪 费了资金， 又对环境造成污染。 For a long time, the liquid chlorination reaction is that the liquid chlorine is heated and vaporized and then introduced into the material from the upper part of the reactor. Due to the internal stirring of the reactor or other reasons, the depth of the chlorine tube inserted into the kettle is limited, so there is always a comparison. The chlorine gas is too late to react and volatilizes and enters the tail gas absorption system together with the hydrogen chloride gas. Due to the presence of more chlorine gas, not only the raw material liquid chlorine is wasted, but also the burden of the exhaust gas absorption system is increased, and the alkali used for exhaust gas absorption is greatly increased. Liquid, which increases the cost of the company's products. Not only does it cause a lot of pollution to the environment, but it also wastes a large part of the resources (liquid chlorine), which costs money and pollutes the environment.
因此， 急需一种改进的技术来解决现有技术中所存在的这一问题。 发明内容 Therefore, there is an urgent need for an improved technique to solve this problem in the prior art. Summary of the invention
本发明提供一种 3， 5-二氯 -4-氨基三氟甲苯通氯方法， 还提供一种应 用于 3， 5-二氯 -4-氨基三氟甲苯通氯方法中的通氯系统。 The present invention provides a 3,5-dichloro-4-aminobenzotrifluoride chloride process, and a chlorine system for use in a 3,5-dichloro-4-aminobenzotrifluoride chloride process.
本发明采用的技术方案是： The technical solution adopted by the invention is:
3， 5-二氯 -4-氨基三氟甲苯通氯方法， 包括以下步骤： The 3, 5-dichloro-4-aminobenzotrifluoride chloride method comprises the following steps:
a、 检査通氯系统各个设备， 调节冷却水， 打开石墨换热器阀门开启真 空按钮， 投入 700-1000质量份的 4-氨基 -三氟甲苯； a. Check the equipment of the chlorine system, adjust the cooling water, open the graphite heat exchanger valve to open the vacuum button, and input 700-1000 parts by mass of 4-amino-trifluorotoluene;
b、 将 4-氨基-三氟甲苯对三氟甲基苯胺泵上吸入对胺计量槽， 放入氯 化釜； b, 4-amino-trifluorotoluene p-trifluoromethylaniline pump is inhaled into the amine metering tank, placed in the chlorination tank;
c、 将 2300-2600质量份的二氯乙垸泵上二氯乙垸高位槽， 放入氯化釜 内， 氯化釜内液位不超过 2/3 体积， 放完后， 关闭进料阔， 并将二氯乙垸
高位槽内多余物料放回原料储槽， 并加入 1200-1400质量份的水； d、 检查各阔门和检查仪表管线， 开蒸气， 当釜温至 33-36 °C时关蒸气， 开始氯化； c. Pump 2300-2600 parts by mass of dichloroacetic acid on the high-level tank of dichloroacetic acid into the chlorination kettle. The liquid level in the chlorination kettle should not exceed 2/3 volume. After the discharge, close the feed width. Dichloroacetamidine The excess material in the high tank is returned to the raw material storage tank, and 1200-1400 mass parts of water are added; d. Check the various wide doors and check the instrument pipeline, open the steam, turn off the steam when the temperature of the kettle reaches 33-36 °C, start chlorine Chemical
e、 打开氯化釜进氯气阀、 输管截止阀、 通氯管针阀、 氯气瓶， 向热水 槽通 650-700质量份的液氯， 通氯速度为 65-70质量份 /小时， 反应温度为 55-60 °C , 当通氯达 650-700 质量份时， 取样分析， 如果反应没合格， 每 10质量份加一次氯气， 当一氯小于 1 %时通氯结束； e. Open the chlorination kettle into the chlorine valve, the pipe shut-off valve, the chlorine pipe needle valve, the chlorine gas bottle, and pass 650-700 parts by mass of liquid chlorine to the hot water tank. The chlorine passing rate is 65-70 mass parts/hour. The temperature is 55-60 °C, when the chlorine reaches 650-700 parts by mass, sample analysis, if the reaction is not qualified, add chlorine gas every 10 parts by mass, when chlorine exceeds 1%, the chlorine is over;
f、 通氯完毕， 关闭氯气瓶、 通氯管针睛、 输氯管截止阀、 流量进出阀 门， 保温 50-70分钟， 静置 25-40分钟， 分出下层有机相， 真空抽 氯化 中间槽， 中间层搜集待下批氯化， 得到 3， 5-二氯 -4-氨基三氟甲苯 水相 排入沉降槽。 f. After the chlorine is completed, close the chlorine gas cylinder, the chlorine pipe needle, the chlorine pipe shut-off valve, the flow inlet and outlet valve, keep the heat for 50-70 minutes, let stand for 25-40 minutes, separate the lower organic phase, and vacuum the chlorination. The trough and the intermediate layer collect the chlorination to be pulverized, and the aqueous phase of 3, 5-dichloro-4-aminobenzotrifluoride is discharged into the settling tank.
3, 5 -二氯- 4 -氨基三三氟甲苯通氯方法中的通氯系统，所述通氯系统包括 多组氯化设备组件， 所述氯化设备组件包括氯化釜、 氯气缓冲罐 、 氯气瓶 和气化器， 所述氯化釜顶部分别连接石墨冷凝器、 对胺计量槽 一氯乙烧 高位槽、 氯气缓冲罐， 所述氯化釜和石墨冷凝器之间设有石墨换热器阀门， 所述氯化釜和氯气缓冲罐之间的通氯管道上靠近氯化釜端设有氯化釜进氯 气阀 ， 所述氯化釜和氯气缓冲罐之间的通氯管道上靠近氯气缓冲罐端设有 输管截止阀， 所述通氯管道上还设有流量进出阔门， 所述氯化釜进氯气阔 和输 截止阀之间设有进料阀， 所述氯 连接气化器， 所述气化器 连接氯气瓶和热水槽， 所述气化器和氯气瓶之间设有通氯管针圆， 所述氯 化釜底部连接氯化中间槽和沉降槽， 所述氯化中间槽底部连接溶剂槽和脱 溶 所述溶剂槽连接二氯乙垸接受槽 ， 所述二氯乙垸接受槽连接石墨冷 凝 所述脱溶釜连接碱洗釜， 所述碱洗釜和脱溶釜之间设有半成品泵。 a chlorine-passing system in a 3,5-dichloro-4-aminotrifluorotoluene chloride process, the chlorine-passing system comprising a plurality of sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle, a chlorine buffer tank a chlorine gas cylinder and a gasifier, wherein the top of the chlorination kettle is respectively connected with a graphite condenser, a high-level tank for a chlorine metering tank of an amine metering tank, a buffer tank for chlorine gas, and a graphite heat exchange between the chlorination tank and the graphite condenser. a chlorine valve in the chlorine passage between the chlorination tank and the chlorine buffer tank is arranged near the chlorination kettle end, and a chlorine inlet valve is arranged on the chlorine passage between the chlorination kettle and the chlorine buffer tank. a chlorine gas buffer tank end is provided with a pipeline cut-off valve, and the chlorine pipeline is further provided with a flow inlet and outlet wide door, and a feed valve is arranged between the chlorine gas inlet and the cut-off valve of the chlorination kettle, and the chlorine connecting gas is arranged a gasifier connected to the chlorine gas bottle and the hot water tank, wherein the gasifier and the chlorine gas bottle are provided with a chlorine tube needle circle, and the bottom of the chlorination kettle is connected with the chlorination intermediate tank and the settling tank, Connecting the solvent tank at the bottom of the chlorination intermediate tank and desolving the solvent tank connection Chloroacetamide embankment receiving groove, the receiving groove dichloroacetyl embankment graphite condenser connected to the desolvation tank connected caustic tank, a pump is provided between the semi-finished product caustic autoclave reactor and desolvation.
本发明的有益效果是： 底部通氯大大节约了液氯的用量， 既节约了原
材料， 减少了尾气吸收所用的液碱， 取得了可观的经济效益， 同时又减少 了对环境的污染， 取得了较好的环境效益。 The beneficial effects of the invention are as follows: the chlorine at the bottom greatly saves the amount of liquid chlorine, which saves the original The material has reduced the liquid alkali used for exhaust gas absorption, and has achieved considerable economic benefits. At the same time, it has reduced environmental pollution and achieved good environmental benefits.
附图说明 DRAWINGS
下面结合附图和具体实施方式对本发明作进一步详细描述。 The present invention will be further described in detail below in conjunction with the drawings and specific embodiments.
图 1为本发明的结构示意图。 Figure 1 is a schematic view of the structure of the present invention.
其中： 1、 氯化釜， 2、 氯气缓冲罐， 3、 氯气瓶， 4、 气化器， 5、 石墨 冷凝器， 6、 对胺计量槽， 7、 二氯乙垸高位槽， 8、 石墨换热器阔门， 9、 氯化釜进氯气阀， 10、 输管截止阀， 11、 进料阀， 12、 热水槽， 13、 通氯 管针闽， 14、 氯化中间槽， 15、 沉降槽， 16、 溶剂槽， 17、 脱溶釜， 18、 二氯乙垸接受槽， 19、 石墨冷凝器， 20、 碱洗釜， 21、 半成品泵， 22、 通 氯管道， 23、 流量进出阔门。 Among them: 1, chlorination kettle, 2, chlorine buffer tank, 3, chlorine gas cylinder, 4, gasifier, 5, graphite condenser, 6, amine metering tank, 7, high-level tank of dichloroacetamidine, 8, graphite Heat exchanger wide door, 9, chlorination kettle into the chlorine valve, 10, the pipe cut-off valve, 11, the feed valve, 12, hot water tank, 13, chlorine tube needle, 14, chlorination tank, 15, Settling tank, 16, solvent tank, 17, desolvent kettle, 18, dichloroacetic acid receiving tank, 19, graphite condenser, 20, alkali washing kettle, 21, semi-finished pump, 22, chlorine pipeline, 23, flow in and out Wide door.
具体实施方式 detailed description
实施例 1 Example 1
如图 1 所示， 本发明的 3， 5-二氯 -4-氨基三氟甲苯通氯方法， 包括以 下步骤： As shown in Fig. 1, the 3,5-dichloro-4-aminobenzotrifluoride chloride method of the present invention comprises the following steps:
a、 检査釜内情况， 关闭釜底阔门， 检査高位槽、 原料槽、 各物料泵阔 门， 使其处于正确位置， 调节冷却水， 打开石墨换热器闽门 8 开启真空按 钮， 投入 700kg的 4-氨基 -三氟甲苯； a. Check the condition of the kettle, close the bottom of the kettle, check the high tank, the material tank, the pump door of each material, make it in the correct position, adjust the cooling water, open the graphite heat exchanger door 8 and open the vacuum button. Inject 700 kg of 4-amino-trifluorotoluene;
b、 将 4-氨基 -三氟甲苯对三氟甲基苯胺泵上吸入对胺计量槽 6， 放入 氯化釜 1; b, 4-amino-trifluorotoluene p-trifluoromethylaniline pump is inhaled into the amine metering tank 6, into the chlorination tank 1;
c、 将 2300kg 的二氯乙烷泵上二氯乙烷高位槽 7， 放入氯化釜 1 内， 氯化釜 1 内液位不超过 2/3体积， 放完后， 关闭进料阀 11， 并将二氯乙垸 高位槽 7 内多余物料放回原料储槽， 并加入 1200kg的水； c. Pump 2300kg of dichloroethane on the dichloroethane high level tank 7 and put it into the chlorination tank 1. The liquid level in the chlorination tank 1 does not exceed 2/3 volume. After the discharge, close the feed valve 11 And returning the excess material in the high-level tank 7 of the dichloroacetic acid back to the raw material storage tank, and adding 1200 kg of water;
d、 检查各阔门和检查仪表管线， 开蒸气， 当釜温至 33'C时关蒸气，
开始氯化； d. Check the wide doors and check the instrument pipelines, open the steam, and turn off the steam when the kettle temperature reaches 33'C. Start chlorination;
e、 打开氯化釜进氯气阔 9、 输管截止阔 10、 通氯管针阔 13、 氯气瓶 3， 向热水槽 12通 650kg的液氯， 通氯速度为 65kg/小时， 反应温度为 55°C， 当通氯达 650kg时， 取样分析， 如果反应没合格， 每 10kg加一次氯气， 当 一氯小于 1 %时通氯结束； e. Open the chlorination kettle to enter the chlorine gas width 9, the outlet pipe width is 10, the chlorine pipe needle width is 13. The chlorine gas bottle 3, and the hot water tank 12 is connected with 650 kg of liquid chlorine. The chlorine passing rate is 65 kg/hour, and the reaction temperature is 55. °C, when the chlorine reaches 650kg, sample analysis, if the reaction is not qualified, add chlorine gas every 10kg, when chlorine is less than 1%, the chlorine will end;
f、 通氯完毕， 关闭氯气瓶 3、 通氯管针阀 13、 输氯管截止阔 10、 流 量进出阔门 23， 保温 50分钟， 静置 25分钟， 分出下层有机相， 真空抽至 氯化中间槽 14， 得到 3， 5-二氯 -4-氨基三氟甲苯， 中间层搜集待下批氯化， 水相排入沉降槽 15。 f. After the chlorine is completed, close the chlorine cylinder 3, the chlorine tube needle valve 13, the chlorine tube cut-off width 10, the flow rate into and out of the wide door 23, keep warm for 50 minutes, let stand for 25 minutes, separate the lower organic phase, vacuum to chlorine The intermediate tank 14 was obtained to obtain 3,5-dichloro-4-aminobenzotrifluoride, and the intermediate layer was collected to be chlorinated in the next batch, and the aqueous phase was discharged into the settling tank 15.
3， 5-二氯 -4-氨基三氟甲苯通氯方法中的通氯系统，所述通氯系统包括 二组氯化设备组件， 所述氯化设备组件包括氯化釜 1、 氯气缓冲罐 2、 氯气 瓶 3和气化器 4， 所述氯化釜 1顶部分别连接石墨冷凝器 5、对胺计量槽 6、 二氯乙垸高位槽 7、 氯气缓冲罐 2， 所述氯化釜 1和石墨冷凝器 5之间设有 石墨换热器阀门 8， 所述氯化釜 1和氯气缓冲罐 2之间的通氯管道 22上靠 近氯化釜 1 端设有氯化釜进氯气阀 9， 所述氯化釜 1 和氯气缓冲罐 2之间 的通氯管道 22 上靠近氯气缓冲罐 2 端设有输管截止阀 10， 所述通氯管道 22上还设有流量进出闽门 23， 所述氯化釜进氯气阔 9和输管截止阀 10之 间设有进料阀 11， 所述氯气缓冲罐 2连接气化器 4， 所述气化器 4连接氯 气瓶 3和热水槽 12， 所述气化器 4和氯气瓶 3之间设有通氯管针阀 13， 所 述氯化釜 1底部连接氯化中间槽 14和沉降槽 15， 所述氯化中间槽 14底部 连接溶剂槽 16和脱溶釜 17， 所述溶剂槽 16连接二氯乙垸接受槽 18， 所述 二氯乙垸接受槽 18连接石墨冷凝器 19， 所述脱溶釜 17连接碱洗釜 20， 所 述碱洗釜 20和脱溶釜 17之间设有半成品泵 21。 a chlorine-passing system in a 3, 5-dichloro-4-aminobenzotrifluoride chloride process, the chlorine-passing system comprising two sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle 1, a chlorine buffer tank 2. a chlorine gas bottle 3 and a gasifier 4, wherein the top of the chlorination kettle 1 is connected to a graphite condenser 5, an amine metering tank 6, a dichloroacetic acid high level tank 7, a chlorine gas buffer tank 2, and the chlorination tank 1 and A graphite heat exchanger valve 8 is disposed between the graphite condenser 5, and a chlorination kettle chlorine gas valve 9 is disposed on the chlorine passage 22 between the chlorination kettle 1 and the chlorine buffer tank 2 near the chlorination tank 1 end. a chlorine outlet pipe 22 between the chlorination tank 1 and the chlorine buffer tank 2 is provided with a pipe shut-off valve 10 near the chlorine buffer tank 2, and the flow passage 22 is further provided with a flow inlet and outlet port 23, A feed valve 11 is disposed between the chlorination kettle chlorine gas 9 and the pipeline shutoff valve 10, and the chlorine buffer tank 2 is connected to the gasifier 4, and the gasifier 4 is connected to the chlorine gas cylinder 3 and the hot water tank 12, A gas chloride needle valve 13 is disposed between the gasifier 4 and the chlorine gas bottle 3, and the bottom of the chlorination kettle 1 is connected to the chlorination. The tank 14 and the settling tank 15, the bottom of the chlorination intermediate tank 14 is connected with a solvent tank 16 and a desolvent tank 17, and the solvent tank 16 is connected to the dichloroacetone receiving tank 18, and the dichloroacetone receiving tank 18 is connected to the graphite. The condenser 19 is connected to the alkali washing tank 20, and a semi-finished pump 21 is disposed between the alkali washing tank 20 and the desolvent tank 17.
实施例 2
如图 1 所示， 本发明的 3， 5-二氯- 4-氨基三氟甲苯通氯方法， 包括以 下步骤： Example 2 As shown in Fig. 1, the 3,5-dichloro-4-aminobenzotrifluoride chloride method of the present invention comprises the following steps:
a、 检查釜内情况， 关闭釜底阀门， 检査高位槽、 原料槽、 各物料泵阔 门， 使其处于正确位置， 调节冷却水， 打开石墨换热器阔门 8 开启真空按 钮， 投入 800kg的 4-氨基 -三氟甲苯； a. Check the condition of the kettle, close the bottom valve, check the high level tank, the material tank, the material pump wide door, make it in the correct position, adjust the cooling water, open the graphite heat exchanger wide door 8 open the vacuum button, put 800kg 4-amino-trifluorotoluene;
b、 将 4-氨基 -三氟甲苯对三氟甲基苯胺泵上吸入对胺计量槽 6， 放入 氯化釜 1; b, 4-amino-trifluorotoluene p-trifluoromethylaniline pump is inhaled into the amine metering tank 6, into the chlorination tank 1;
c、 将 2500kg 的二氯乙垸泵上二氯乙垸高位槽 7， 放入氯化釜 1 内， 氯化釜 1 内液位不超过 2/3体积， 放完后， 关闭进料阀 11， 并将二氯乙垸 高位槽 7 内多余物料放回原料储槽， 并加入 1250kg的水； c. Pump 2500kg of dichloroacetic acid on the high-level tank of dichloroacetic acid, and put it into the chlorination tank 1. The liquid level in the chlorination tank 1 does not exceed 2/3 volume. After the discharge, close the feed valve 11 , and put the excess material in the high-level tank 7 of the dichloroacetate back into the raw material storage tank, and add 1250 kg of water;
d、 检査各阔门和检查仪表管线， 开蒸气， 当釜温至 35Ό时关蒸气， 开始氯化； d. Check the wide doors and check the instrument pipelines, open the steam, turn off the steam when the temperature of the kettle reaches 35 ,, start chlorination;
e、 打开氯化釜进氯气阔 9、 输管截止阔 10、 通氯管针阔 13、 氯气瓶 3， 向热水槽 12通 680kg的液氯， 通氯速度为 68kg/小时， 反应温度为 58°C， 当通氯达 660kg时， 取样分析， 如果反应没合格， 每 10kg加一次氯气， 当 一氯小于 1 %时通氯结束； e. Open the chlorination kettle to enter the chlorine gas width 9, the outlet pipe width is 10, the chlorine pipe needle width is 13. The chlorine gas bottle 3, and the hot water tank 12 is connected with 680 kg of liquid chlorine. The chlorine passing rate is 68 kg/hour, and the reaction temperature is 58. °C, when the chlorine reaches 660kg, sample analysis, if the reaction is not qualified, add chlorine gas every 10kg, when the chlorine is less than 1%, the chlorine will end;
f、 通氯完毕， 关闭氯气瓶 3、 通氯管针阀 13、 输氯管截止阔 10、 流 量进出阔门 23， 保温 60分钟， 静置 30分钟， 分出下层有机相， 真空抽至 氯化中间槽 14， 中间层搜集待下批氯化， 得到 3， 5-二氯 -4-氨基三氟甲苯， 水相排入沉降槽 15。 f. After the chlorine is completed, close the chlorine cylinder 3, the chlorine tube needle valve 13, the chlorine tube cut-off width 10, the flow rate into and out of the wide door 23, keep warm for 60 minutes, let stand for 30 minutes, separate the lower organic phase, vacuum pump to chlorine The intermediate tank 14 is collected, and the intermediate layer collects the chlorination to be pulverized to obtain 3,5-dichloro-4-aminobenzotrifluoride, and the aqueous phase is discharged into the settling tank 15.
3， 5-二氯 -4-氨基三氟甲苯通氯方法中的通氯系统，所述通氯系统包括 二组氯化设备组件， 所述氯化设备组件包括氯化釜 1、 氯气缓冲罐 2、 氯气 瓶 3和气化器 4， 所述氯化釜 1顶部分别连接石墨冷凝器 5、对胺计量槽 6、 二氯乙垸高位槽 7、 氯气缓冲罐 2， 所述氯化釜 1和石墨冷凝器 5之间设有
石墨换热器阀门 8， 所述氯化釜 1和氯气缓冲罐 2之间的通氯管道 22上靠 近氯化釜 1 端设有氯化釜进氯气阔 9， 所述氯化釜 1 和氯气缓冲罐 2之间 的通氯管道 22 上靠近氯气缓冲罐 2 端设有输管截止阀 10， 所述通氯管道 22上还设有流量进出阔门 23， 所述氯化釜进氯气陶 9和输管截止阀 10之 间设有进料阀 11， 所述氯气缓冲罐 2连接气化器 4， 所述气化器 4连接氯 气瓶 3和热水槽 12， 所述气化器 4和氯气瓶 3之间设有通氯管针阀 13， 所 述氯化釜 1底部连接氯化中间槽 14和沉降槽 15， 所述氯化中间槽 14底部 连接溶剂槽 16和脱溶釜 17， 所述溶剂槽 16连接二氯乙垸接受槽 18， 所述 二氯乙垸接受槽 18连接石墨冷凝器 19， 所述脱溶釜 17连接碱洗釜 20， 所 述碱洗釜 20和脱溶釜 17之间设有半成品泵 21。 a chlorine-passing system in a 3, 5-dichloro-4-aminobenzotrifluoride chloride process, the chlorine-passing system comprising two sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle 1, a chlorine buffer tank 2. a chlorine gas bottle 3 and a gasifier 4, wherein the top of the chlorination kettle 1 is connected to a graphite condenser 5, an amine metering tank 6, a dichloroacetic acid high level tank 7, a chlorine gas buffer tank 2, and the chlorination tank 1 and Between the graphite condenser 5 a graphite heat exchanger valve 8, a chlorine gas pipe 22 between the chlorination kettle 1 and the chlorine buffer tank 2 is disposed near the chlorination tank 1 and is provided with a chlorination kettle into the chlorine gas 9, the chlorination kettle 1 and chlorine gas A chlorine shut-off valve 10 is disposed on the chlorine-passing pipe 22 between the buffer tanks 2 near the chlorine buffer tank 2, and a flow-in and out-out valve 23 is further disposed on the chlorine-passing pipe 22, and the chlorination kettle enters the chlorine gas pottery 9 A feed valve 11 is disposed between the line shutoff valve 10 and the chlorine buffer tank 2 is connected to the gasifier 4, and the gasifier 4 is connected to a chlorine gas bottle 3 and a hot water tank 12, the gasifier 4 and chlorine gas. A chlorine tube needle valve 13 is disposed between the bottles 3, and the bottom of the chlorination tank 1 is connected with a chlorination intermediate tank 14 and a settling tank 15, and the bottom of the chlorination intermediate tank 14 is connected with a solvent tank 16 and a desolvent tank 17, The solvent tank 16 is connected to the dichloroacetone receiving tank 18, and the dichloroacetone receiving tank 18 is connected to the graphite condenser 19, and the desolvent tank 17 is connected to the alkali washing tank 20, the alkali washing tank 20 and the desolvent kettle. A semi-finished product pump 21 is provided between the 17th.
实施例 3 Example 3
如图 1 所示， 本发明的 3， 5-二氯- 4-氨基三氟甲苯通氯方法， 包括以 下步骤： As shown in Fig. 1, the 3,5-dichloro-4-aminobenzotrifluoride chloride method of the present invention comprises the following steps:
a、 检查釜内情况， 关闭釜底闽门， 检査高位槽、 原料槽、 各物料泵阀 门， 使其处于正确位置， 调节冷却水， 打开石墨换热器阔门 8 开启真空按 钮， 投入 850kg的 4-氨基 -三氟甲苯； a. Check the inside of the kettle, close the bottom of the kettle, check the high tank, the material tank, the pump valves of each material, make them in the correct position, adjust the cooling water, open the graphite heat exchanger, open the door, open the vacuum button, and put in 850 kg of 4-amino-trifluorotoluene;
b、 将 4-氨基 -三氟甲苯对三氟甲基苯胺泵上吸入对胺计量槽 6， 放入 氯化釜 1; b, 4-amino-trifluorotoluene p-trifluoromethylaniline pump is inhaled into the amine metering tank 6, into the chlorination tank 1;
c、 将 2600kg 的二氯乙垸泵上二氯乙垸高位槽 7， 放入氯化釜 1 内， 氯化釜 1 内液位不超过 2/3体积， 放完后， 关闭进料阀 11， 并将二氯乙垸 高位槽 7 内多余物料放回原料储槽， 并加入 1350kg的水； c. Pump 2600kg of dichloroacetic acid on the dichloroacetic acid high level tank 7 and put it into the chlorination tank 1. The liquid level in the chlorination tank 1 does not exceed 2/3 volume. After the discharge, close the feed valve 11 , and put the excess material in the high-level tank 7 of the dichloroacetate back into the raw material storage tank, and add 1350 kg of water;
d、 检査各阔门和检查仪表管线， 开蒸气， 当釜温至 36Ό时关蒸气， 开始氯化； d. Check the wide doors and check the instrument pipelines, open the steam, turn off the steam when the kettle temperature reaches 36 ,, start chlorination;
e、 打开氯化釜进氯气阔 9、 输管截止阔 10、 通氯管针阔 13、 氯气瓶 3，
向热水槽 12通 700kg的液氯， 通氯速度为 70kg/小时， 反应温度为 60°C， 当通氯达 680kg时， 取样分析， 如果反应没合格， 每 10kg加一次氯气， 当 一氯小于 1 %时通氯结束； e. Open the chlorination kettle to enter the chlorine gas width 9, the outlet pipe width is 10, the chlorine pipe needle width is 13, the chlorine gas bottle 3, 700 kg of liquid chlorine is supplied to the hot water tank 12, the chlorine passing rate is 70 kg/hour, the reaction temperature is 60 ° C, and when the chlorine is 680 kg, sampling and analysis is performed. If the reaction is not qualified, chlorine gas is added once every 10 kg, when the chlorine is less than At 1%, the chlorine is over;
f、 通氯完毕， 关闭氯气瓶 3、 通氯管针阔 13、 输氯管截止阀 10、 流 量进出阀门 23， 保温 65分钟， 静置 32分钟， 分出下层有机相， 真空抽至 氯化中间槽 14， 中间层搜集待下批氯化， 得到 3， 5-二氯 -4-氨基三氟甲苯， 水相排入沉降槽 15。 f. After the chlorine is completed, close the chlorine gas bottle 3, the chlorine tube needle width 13, the chlorine tube shut-off valve 10, the flow inlet and outlet valve 23, keep warm for 65 minutes, let stand for 32 minutes, separate the lower organic phase, vacuum pump to chlorinate In the intermediate tank 14, the intermediate layer collects the chlorination to be batched to obtain 3,5-dichloro-4-aminobenzotrifluoride, and the aqueous phase is discharged into the settling tank 15.
3, 5-二氯 -4-氨基三氟甲苯通氯方法中的通氯系统，所述通氯系统包括 二组氯化设备组件， 所述氯化设备组件包括氯化釜 1、 氯气缓冲罐 2、 氯气 瓶 3和气化器 4， 所述氯化釜 1顶部分别连接石墨冷凝器 5、对胺计量槽 6、 二氯乙垸高位槽 7、 氯气缓冲罐 2， 所述氯化釜 1和石墨冷凝器 5之间设有 石墨换热器阀门 8， 所述氯化釜 1和氯气缓冲罐 2之间的通氯管道 22上靠 近氯化釜 1 端设有氯化釜进氯气阔 9， 所述氯化釜 1 和氯气缓冲罐 2之间 的通氯管道 22 上靠近氯气缓冲罐 2 端设有输管截止阀 10， 所述通氯管道 22上还设有流量进出阔门 23， 所述氯化釜进氯气陶 9和输管截止阀 10之 间设有进料阀 11， 所述氯气缓冲罐 2连接气化器 4， 所述气化器 4连接氯 气瓶 3和热水槽 12， 所述气化器 4和氯气瓶 3之间设有通氯管针阀 13， 所 述氯化釜 1底部连接氯化中间槽 14和沉降槽 15， 所述氯化中间槽 14底部 连接溶剂槽 16和脱溶釜 17， 所述溶剂槽 16连接二氯乙垸接受槽 18， 所述 二氯乙垸接受槽 18连接石墨冷凝器 19， 所述脱溶釜 17连接碱洗釜 20， 所 述碱洗釜 20和脱溶釜 17之间设有半成品泵 21。 a chlorine-passing system in a 3, 5-dichloro-4-aminobenzotrifluoride chloride process, the chlorine-passing system comprising two sets of chlorination equipment components, the chlorination plant component comprising a chlorination kettle 1, a chlorine buffer tank 2. a chlorine gas bottle 3 and a gasifier 4, wherein the top of the chlorination kettle 1 is connected to a graphite condenser 5, an amine metering tank 6, a dichloroacetic acid high level tank 7, a chlorine gas buffer tank 2, and the chlorination tank 1 and A graphite heat exchanger valve 8 is disposed between the graphite condensers 5, and a chlorination tank is provided with a chlorine gas 9 on the chlorine passage 22 between the chlorination tank 1 and the chlorine buffer tank 2, near the chlorination tank 1 end. A chlorine shut-off valve 10 is disposed on the chlorine-passing pipe 22 between the chlorination tank 1 and the chlorine buffer tank 2 near the chlorine buffer tank 2, and the gas-passing pipe 22 is further provided with a flow inlet and outlet door 23, A feed valve 11 is disposed between the chlorination kettle and the gas shutoff valve 10, and the chlorine buffer tank 2 is connected to the gasifier 4, and the gasifier 4 is connected to the chlorine gas bottle 3 and the hot water tank 12, A gas chloride needle valve 13 is disposed between the gasifier 4 and the chlorine gas cylinder 3, and the bottom of the chlorination kettle 1 is connected to the middle of the chlorination. 14 and a settling tank 15, wherein the bottom of the chlorination intermediate tank 14 is connected to a solvent tank 16 and a desolvent tank 17, the solvent tank 16 is connected to a dichloroacetone receiving tank 18, and the dichloroacetone receiving tank 18 is connected to graphite condensation. The desolvent tank 17 is connected to the alkali washing tank 20, and a semi-finished product pump 21 is disposed between the alkali washing tank 20 and the desolvent tank 17.
底部通氯大大节约了液氯的用量， 既节约了原材料， 减少了尾气吸收 所用的液碱， 取得了可观的经济效益， 同时又减少了对环境的污染， 取得 了较好的环境效益。
The chlorine at the bottom greatly saves the amount of liquid chlorine, which not only saves raw materials, but also reduces the liquid alkali used for exhaust gas absorption, and has achieved considerable economic benefits. At the same time, it has reduced environmental pollution and achieved good environmental benefits.
Claims
1、 3， 5-二氯- 4-氨基三氟甲苯通氯方法， 其特征在于包括以下步骤： a、 检查通氯系统各个设备， 调节冷却水， 打开石墨换热器阔门开启真 空按钮， 投入 700-1000质量份的 4-氨基 -三氟甲苯； 1. The chlorination method for 3, 5-dichloro-4-aminotrifluorotoluene is characterized by including the following steps: a. Check each equipment of the chlorination system, adjust the cooling water, open the wide door of the graphite heat exchanger and turn on the vacuum button, Put in 700-1000 parts by mass of 4-amino-trifluorotoluene;
b、 将 4-氨基-三氟甲苯对三氟甲基苯胺泵上吸入对胺计量槽， 放入氯 化釜； b. Pump 4-amino-trifluorotoluene-p-trifluoromethylaniline into the amine metering tank and put it into the chlorination kettle;
c、 将 2300-2600质量份的二氯乙烷泵上二氯乙烷高位槽， 放入氯化釜 内， 氯化釜内液位不超过 2/3 体积， 放完后， 关闭进料阀， 并将二氯乙烷 高位槽内多余物料放回原料储槽， 并加入 1200-1400质量份的水； c. Pump 2300-2600 parts by mass of dichloroethane into the dichloroethane high-level tank and put it into the chlorination kettle. The liquid level in the chlorination kettle should not exceed 2/3 of the volume. After placing it, close the feed valve. , and return the excess material in the dichloroethane high-level tank to the raw material storage tank, and add 1200-1400 parts by mass of water;
d、 检查各阀门和检查仪表管线， 开蒸气， 当釜温至 33-36 °C时关蒸气， 开始氯化； d. Check each valve and instrument pipeline, turn on the steam, turn off the steam when the kettle temperature reaches 33-36 °C, and start chlorination;
e、 打开氯化釜进氯气阀、 输管截止阔、 通氯管针阀、 氯气瓶， 向热水 槽通 650-700质量份的液氯， 通氯速度为 65-70质量份 /小时， 反应温度为 55-60 °C , 当通氯达 650-700 质量份时， 取样分析， 如果反应没合格， 每 10质量份加一次氯气， 当一氯小于 1 %时通氯结束； e. Open the chlorine gas inlet valve, pipeline cut-off valve, chlorine pipe needle valve, and chlorine gas bottle, and pass 650-700 parts by mass of liquid chlorine to the hot water tank at a chlorine flow rate of 65-70 parts by mass/hour. Reaction The temperature is 55-60 °C. When the chlorine reaches 650-700 parts by mass, take a sample for analysis. If the reaction fails, add chlorine once every 10 parts by mass. When the chlorine is less than 1%, the chlorine flow ends;
f、 通氯完毕， 关闭氯气瓶、 通氯管针阀、 输氯管截止阀、 流量进出陶 门， 保温 50-70分钟， 静置 25-40分钟， 分出下层有机相， 真空抽至氯化 中间槽， 得到 3， 5-二氯 -4-氨基三氟甲苯， 中间层搜集待下批氯化， 水相 排入沉降槽。 f. After the chlorine flow is completed, close the chlorine gas bottle, the needle valve of the chlorine pipe, the stop valve of the chlorine pipe, and the flow in and out pottery door, keep it warm for 50-70 minutes, let it stand for 25-40 minutes, separate the lower organic phase, and vacuum to remove the chlorine Chemicalize the intermediate tank to obtain 3, 5-dichloro-4-aminotrifluorotoluene. The intermediate layer is collected for the next batch of chlorination, and the aqueous phase is discharged into the settling tank.
2、 根据权利要求 1所述的 3, 5-二氯 -4-氨基三氟甲苯通氯方法中的通氯系 统， 其特征在于： 所述通氯系统包括氯化设备组件， 所述氯化设备组件包 括氯化釜、 氯气缓冲罐、 氯气瓶和气化器， 所述氯化釜顶部分别连接石墨 冷凝器、 对胺计量槽、 二氯乙垸高位槽、 氯气缓冲罐， 所述氯化釜和石墨 冷凝器之间设有石墨换热器阀门， 所述氯化釜和氯气缓冲罐之间的通氯管 道上靠近氯化釜端设有氯化釜进氯气阀， 所述氯化釜和氯气缓冲罐之间的
通氯管道上靠近氯气缓冲 端设有输管截止阔， 所述通氯管道上还设有流 量进出阔门， 所述氯化釜进氯气阀和输管截止阔之间设有进料阔 ， 所述氯 气缓冲 连接气化器， 所述气化器连接氯气瓶和热水槽， 所述气化器和氯 气瓶之间设有通氯管针陶 ， 所述氯化釜底部连接氯化中间槽和沉降槽 ， 所 述氯化中间槽底部连接溶剂槽和脱溶釜，所述溶剂槽连接二氯乙垸接受槽， 所述二氯乙烷接受槽连接石墨冷凝器， 所述脱溶釜连接碱洗釜， 所述碱洗 釜和脱溶釜之间设有半成品泵。
2. The chlorination system in the chlorination method for 3,5-dichloro-4-aminotrifluorotoluene according to claim 1, characterized in that: the chlorination system includes chlorination equipment components, and the chlorination The equipment components include a chlorination kettle, a chlorine buffer tank, a chlorine bottle and a vaporizer. The top of the chlorination kettle is connected to a graphite condenser, an amine metering tank, a dichloroethane high-level tank, and a chlorine buffer tank. The chlorination kettle is connected to the top. A graphite heat exchanger valve is provided between the chlorination kettle and the graphite condenser. A chlorine kettle inlet valve is provided on the chlorine pipeline between the chlorination kettle and the chlorine buffer tank near the chlorination kettle. The chlorination kettle and between chlorine buffer tanks The chlorine pipeline is provided with a pipeline cut-off valve near the chlorine gas buffer end. The chlorine pipeline is also provided with a flow inlet and outlet gate. There is a feed valve between the chlorine gas inlet valve of the chlorination kettle and the pipeline cut-off valve. The chlorine buffer is connected to a vaporizer, the vaporizer is connected to a chlorine bottle and a hot water tank, a chlorine pipe is provided between the vaporizer and the chlorine bottle, and the bottom of the chlorination kettle is connected to a chlorination intermediate tank. and a settling tank, the bottom of the chlorination intermediate tank is connected to a solvent tank and a desolvent kettle, the solvent tank is connected to a dichloroethane receiving tank, the dichloroethane receiving tank is connected to a graphite condenser, and the desolvating kettle is connected to Alkali washing kettle, a semi-finished product pump is provided between the alkali washing kettle and the desolventizing kettle.
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| CN201310399488.5 | 2013-09-05 | ||
| CN201310399488.5A CN103450030B (en) | 2013-09-05 | 2013-09-05 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
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| CN103450030B (en) * | 2013-09-05 | 2015-05-27 | 南通市海圣药业有限公司 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
| WO2015125155A1 (en) * | 2014-02-19 | 2015-08-27 | Srf Limited | Process for the preparation of 2,6-dihalo-para-trifluoromethyl- anilines as intermediates of pyrazoles |
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| EP1528052A1 (en) * | 2003-10-29 | 2005-05-04 | FINCHIMICA S.p.A. | Process for the production of 4-amino-3,5-dichlorobenzotrifluoride with high purity commercial products being obtained in parallel |
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| CN103450030A (en) * | 2013-09-05 | 2013-12-18 | 南通市海圣药业有限公司 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
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| CN100534975C (en) * | 2007-10-16 | 2009-09-02 | 南通市东昌化工有限公司 | Method for producing 2,6-dichloro-4-trifluoromethylaniline |
| CN101423480A (en) * | 2008-11-27 | 2009-05-06 | 苏州市罗森助剂有限公司 | Production method of 2, 6-dichloro-p-nitroaniline and special reaction kettle thereof |
| CN101538206B (en) * | 2009-04-27 | 2012-07-25 | 浙江工业大学 | Method for processing and utilizing trifluoromethyl aniline distillation still residue |
| CN102126747B (en) * | 2011-03-28 | 2012-11-14 | 柳州百韧特先进材料有限公司 | Chlorine introducing method and device for producing stannous chloride by liquid chlorine |
| CN102863342A (en) * | 2012-10-17 | 2013-01-09 | 湖北美天生物科技有限公司 | Preparation method of high-purity 2, 6-dichloro-4-trifluoromethyl aniline |
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| US4388472A (en) * | 1979-07-18 | 1983-06-14 | Imperial Chemical Industries Plc | Substituted diphenyl ethers |
| EP1528052A1 (en) * | 2003-10-29 | 2005-05-04 | FINCHIMICA S.p.A. | Process for the production of 4-amino-3,5-dichlorobenzotrifluoride with high purity commercial products being obtained in parallel |
| CN101289400A (en) * | 2008-03-24 | 2008-10-22 | 浙江巍华化工有限公司 | Process for synthesizing 2,6- dichlor-4-trifluoromethyl aniline |
| CN102701996A (en) * | 2012-05-29 | 2012-10-03 | 吴江市屯村颜料厂 | A method for preparing 3-chloro-4-methylaniline |
| CN103450030A (en) * | 2013-09-05 | 2013-12-18 | 南通市海圣药业有限公司 | Chlorine introducing method of 3,5-dichloro-4-aminotrifluorotoluene and chlorine introducing system applied to chlorine introducing method |
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