CN107827703A - A kind of method and device of tower continuous chlorination production dichlorotoleune - Google Patents
A kind of method and device of tower continuous chlorination production dichlorotoleune Download PDFInfo
- Publication number
- CN107827703A CN107827703A CN201711166007.0A CN201711166007A CN107827703A CN 107827703 A CN107827703 A CN 107827703A CN 201711166007 A CN201711166007 A CN 201711166007A CN 107827703 A CN107827703 A CN 107827703A
- Authority
- CN
- China
- Prior art keywords
- tower
- liquid
- chlorine
- dichlorotoleune
- chlorated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 70
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 29
- 239000000460 chlorine Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 8
- 239000002912 waste gas Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 2,4 di chloro toluene 2,3 dichloro toluene Chemical compound 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010523 cascade reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 210000003722 extracellular fluid Anatomy 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C07C17/12—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the ring of aromatic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method and device of tower continuous chlorination production dichlorotoleune, raw material ortho-chlorotolu'ene and solid powder th-1 catalyst are mixing uniformly to form configuration liquid, it is sent into by tower reactor bottom in tower reactor, simultaneously, chlorine being continuously passed through into tower reactor from tower reactor bottom and carrying out chlorination reaction, gained chlorated liquid is 25 ~ 40 DEG C through outer circulation heat exchanger cooling controlling reaction temperature；When the conversion ratio of the raw material ortho-chlorotolu'ene in chlorated liquid reaches 45% ~ 75%, and 2, when 6 dichlorotoleune selectively reach more than 25%, by chlorated liquid part continuous discharge, at the same time, it is continuous to be passed through configuration liquid, and ensure that be passed through configuration liquid measure is slightly less than load, this rational technology, high income, production capacity is big, and device is simple, and cost of investment is low.
Description
Technical field
The present invention relates to a kind of method and device of tower continuous chlorination production dichlorotoleune.
Background technology
Dichlorotoleune is important fine chemical material, can be widely used in manufacture bactericide, Insecticides (tech) ＆ Herbicides (tech), dye
Material and pigment, medicine and other chemical products, its status and effect have been to be concerned by more and more people, the difficulty of its synthetic technology
And extensive purposes so that the compound produces higher added value, and chlorination industry is mostly with intermittent reaction now
Based on, technique falls behind, and energy and material consumption is high.
The content of the invention
The invention provides a kind of rational technology, high income, production capacity is big, is that the chlorination of raw material continuous catalysis is given birth to ortho-chlorotolu'ene
The method for producing dichlorotoleune.
In order to solve the above problems, the technical solution adopted in the present invention is a kind of such, tower continuous chlorination production
The method of dichlorotoleune, raw material ortho-chlorotolu'ene and solid powder th-1 catalyst are mixing uniformly to form configuration liquid, by tower reaction
Device bottom is sent into tower reactor, meanwhile, continuously it is passed through chlorine into tower reactor from tower reactor bottom and carries out chlorine
Change reaction, gained chlorated liquid is 25 ~ 40 DEG C through outer circulation heat exchanger cooling controlling reaction temperature；When the raw material in chlorated liquid is adjacent
The conversion ratio of chlorotoluene reaches 45% ~ 75%, and when 2,6-DCT selectively reaches more than 25%, chlorated liquid part is continuous
Discharging, at the same time, configuration liquid is continuously passed through, and ensures that be passed through configuration liquid measure is slightly less than load.
Preferably, the tail gas after chlorination reaction out enters absorption tower at the top of tower reactor, is configured liquid secondary counter
It should absorb after removing chlorine, then through alkali liquor absorption except de-chlorine hydride heel row is put.
Preferably, it is 100 ~ 300 to configure the mass ratio of ortho-chlorotolu'ene and solid powder th-1 catalyst in liquid, wherein, it is described
Solid powder th-1 catalyst is Ti, Sn, Zr, W, AL and Fe chloride, preferably alchlor and ferric trichloride.
Preferably, the flow of chlorine is depending on reaction rate, is the conversion ratio of raw material ortho-chlorotolu'ene in 5% ~ 8%/h
Flow.
The present invention also provides a kind of device of tower continuous chlorination production dichlorotoleune, including reacted for continuous chlorination
Tower reactor, for removing the absorption tower of chlorine in tail gas, for removing in tail gas the spray column of chlorine and matching somebody with somebody for being formed
The configured slot of liquid is put, described tower reactor bottom is provided with configuration liquid feed pipe, the configuration liquid feed pipe and configured slot phase
Even, it is provided with measuring pump on described configuration liquid feed pipe；Described tower reactor top is provided with chlorated liquid discharging opening, institute
The chlorated liquid discharging opening stated is connected with chlorated liquid efferent duct, and described chlorated liquid efferent duct is connected with chlorated liquid outer circulating tube, institute
The chlorated liquid outer circulating tube stated is connected with tower reactor bottom, and described chlorated liquid efferent duct is connected with discharge nozzle, described
Heat exchanger and circulating pump are provided with chlorated liquid outer circulating tube, the chlorated liquid input pipe is connected with chlorine inlet pipe；Described tower
Formula reactor head is provided with waste gas outlet pipe, and the waste gas outlet pipe is connected with the air inlet of absorb the bottom of the tower, and absorb the bottom of the tower goes out
Gas port is connected with the air inlet of spray column, and the inlet on described absorption tower is connected with configured slot.
Preferably, it is provided with chlorine flowrate regulating valve on described chlorine inlet pipe.
Preferably, it is provided with liquid flow control valve on described discharge nozzle
Wherein, in conversion ratio=raw material of raw material ortho-chlorotolu'ene in quality-product of ortho-chlorotolu'ene ortho-chlorotolu'ene quality/raw material
The quality of middle ortho-chlorotolu'ene；
The quality of 2,6- dichlorotoleune selectivity=raw materials ortho-chlorotolu'ene conversion 2,6- dichlorotoleune/（The matter of ortho-chlorotolu'ene in raw material
The quality of ortho-chlorotolu'ene in amount-product）；
Beneficial effect：1st, chlorated liquid is entered tower reactor system by the present invention after reactor external application heat exchanger is cooled down
System cooling, controlling reaction temperature is at 25 ~ 35 DEG C.Secondly, continuous feed and discharging are realized using this process conditions, production capacity is big, production
Product high income, rational technology, chlorine utilization is high, and exhaust emissions is up to standard.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, should
Embodiment is only used for explaining the present invention, is not intended to limit the scope of the present invention..
Embodiment 1
A kind of device of tower continuous chlorination production dichlorotoleune, including for the tower reactor 1 that continuous chlorination reacts, be used for
The absorption tower 2 of chlorine in tail gas, the spray column 3 for removing chlorine in tail gas and the configured slot 4 for forming configuration liquid are removed,
Described tower reactor bottom is provided with configuration liquid feed pipe 5, and the configuration liquid feed pipe 5 is connected with configured slot 4, and described matches somebody with somebody
Put and be provided with measuring pump on liquid feed pipe；Described tower reactor top is provided with chlorated liquid discharging opening, described chlorated liquid
Discharging opening is connected with chlorated liquid efferent duct, and described chlorated liquid efferent duct is connected with chlorated liquid outer circulating tube, described chlorated liquid
Outer circulating tube is connected with tower reactor bottom, and described chlorated liquid efferent duct is connected with discharge nozzle 6, is followed outside described chlorated liquid
Heat exchanger 7 and circulating pump 8 are provided with endless tube, the chlorated liquid input pipe is connected with chlorine inlet pipe 9；Described tower reaction
The top of device 2 is provided with waste gas outlet pipe, and the waste gas outlet pipe is connected with the air inlet of the bottom of absorption tower 2, the gas outlet of the bottom of absorption tower 2
It is connected with the air inlet of spray column 3, the inlet on described absorption tower 2 is connected with configured slot 4.
Wherein, it is provided with chlorine flowrate regulating valve on described chlorine inlet pipe；Liquid flow is provided with described discharge nozzle
Control valve
Embodiment 2
By 55kg ortho-chlorotolu'ene and 203 g ferric trichlorides（Catalyst）Put into make-up tank and stir half an hour formation configuration
Liquid, will then configure that liquid is defeated to be sent into tower reaction tower by feed pipe with measuring pump, be then turned on circulating pump and circulated, be beaten
Open chlorine flowrate regulating valve and lead to chlorine, chlorine flowrate 0.3m3/h, when reaction temperature reaches 20 DEG C, drive heat exchanger and cooled down
Water circulation cools down chlorated liquid, and appropriate chlorine flowrate and the cooler cooling water aperture controlling reaction temperature of adjusting is at 25 ~ 40 DEG C, reaction
About 11 hours time, the gross mass for detecting interstitial fluid in reaction is 62kg, and composition is as shown in table 1 below：
Table 1
| Composition | Ortho-chlorotolu'ene | 2,6- dichlorotoleune | 2,5- dichlorotoleune | 2,4 di chloro toluene | 2,3 dichloro toluene |
| Accounting（w/w） | 59.56% | 11.94% | 13.72% | 7.19% | 5.86% |
The conversion ratio for being computed raw material ortho-chlorotolu'ene reaches 32.8%, and 2,6-DCT selectively reaches 31%, now,
25Kg ortho-chlorotolu'enes and 90g ferric trichlorides are added in configured slot（Catalyst）Stir, with measuring pump with 8L/h speed
Discharged from reaction tower bottom feed, while with 8.1L/h, the composition to be discharged in tandem reaction sequence is as shown in table 2 below：
Table 2
| Composition | Ortho-chlorotolu'ene | 2,6- dichlorotoleune | 2,5- dichlorotoleune | 2,4 di chloro toluene | 2,3 dichloro toluene |
| Accounting（w/w） | 58.79% | 12.27% | 13.07% | 7.29% | 5.83% |
Tail gas after chlorination reaction out enters absorption tower at the top of tower reactor by the air inlet of the bottom on absorption tower, together
When the inlet that top of the liquid through absorption tower is configured in configured slot entered into absorption tower, tail gas is configured the absorption of liquid secondary response and removed
After removing chlorine, the air inlet for entering back into spray tower bottom enters spray column, by spray tower top after alkali liquor absorption removes de-chlorine hydride
The gas outlet discharge in portion, after testing, the tail gas discharged by the gas outlet at the top of spray column meets discharge standard.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (7)
- A kind of 1. method of tower continuous chlorination production dichlorotoleune, it is characterised in that by raw material ortho-chlorotolu'ene and solid powder Catalyst is mixing uniformly to form configuration liquid, is sent into by tower reactor bottom in tower reactor, meanwhile, by tower reactor Bottom is continuously passed through chlorine into tower reactor and carries out chlorination reaction, and gained chlorated liquid is cooled down through outer circulation heat exchanger and controlled Reaction temperature is 25 ~ 40 DEG C；When the conversion ratio of the raw material ortho-chlorotolu'ene in chlorated liquid reaches 45% ~ 75%, and 2,6-DCT When selectivity reaches more than 25%, by chlorated liquid part continuous discharge, at the same time, configuration liquid is continuously passed through, and ensure to be passed through Configuration liquid measure be load 95% ~ 98%.
- 2. the method for a kind of tower continuous chlorination production dichlorotoleune according to claim 1, it is characterised in that chlorination is anti- Tail gas after answering out enters absorption tower at the top of tower reactor, after being configured liquid secondary response absorption removing chlorine, then passes through Alkali liquor absorption is put except de-chlorine hydride heel row.
- A kind of 3. method of tower continuous chlorination production dichlorotoleune according to claim 1, it is characterised in that configuration liquid The mass ratio of middle ortho-chlorotolu'ene and solid powder th-1 catalyst is 100 ~ 300.
- 4. the method for a kind of tower continuous chlorination production dichlorotoleune according to claim 1, it is characterised in that chlorine Flow is flow of the conversion ratio of raw material ortho-chlorotolu'ene in 5% ~ 8%/h depending on reaction rate.
- 5. a kind of device of tower continuous chlorination production dichlorotoleune, it is characterised in that including the tower reacted for continuous chlorination Formula reactor, for removing the absorption tower of chlorine in tail gas, for removing in tail gas the spray column of chlorine and being configured for being formed The configured slot of liquid, described tower reactor bottom are provided with configuration liquid feed pipe, the configuration liquid feed pipe and configured slot phase Even, it is provided with measuring pump on described configuration liquid feed pipe；Described tower reactor top is provided with chlorated liquid discharging opening, institute The chlorated liquid discharging opening stated is connected with chlorated liquid efferent duct, and described chlorated liquid efferent duct is connected with chlorated liquid outer circulating tube, institute The chlorated liquid outer circulating tube stated is connected with tower reactor bottom, and described chlorated liquid efferent duct is connected with discharge nozzle, described Heat exchanger and circulating pump are provided with chlorated liquid outer circulating tube, the chlorated liquid input pipe is connected with chlorine inlet pipe；Described tower Formula reactor head is provided with waste gas outlet pipe, and the waste gas outlet pipe is connected with the air inlet of absorb the bottom of the tower, and absorb the bottom of the tower goes out Gas port is connected with the air inlet of spray column, and the inlet on described absorption tower is connected with configured slot.
- 6. the device of a kind of tower continuous chlorination production dichlorotoleune according to claim 5, it is characterised in that described Chlorine flowrate regulating valve is provided with chlorine inlet pipe.
- 7. the device of a kind of tower continuous chlorination production dichlorotoleune according to claim 5, it is characterised in that described Liquid flow control valve is provided with discharge nozzle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711166007.0A CN107827703A (en) | 2017-11-21 | 2017-11-21 | A kind of method and device of tower continuous chlorination production dichlorotoleune |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711166007.0A CN107827703A (en) | 2017-11-21 | 2017-11-21 | A kind of method and device of tower continuous chlorination production dichlorotoleune |
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| Publication Number | Publication Date |
|---|---|
| CN107827703A true CN107827703A (en) | 2018-03-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711166007.0A Pending CN107827703A (en) | 2017-11-21 | 2017-11-21 | A kind of method and device of tower continuous chlorination production dichlorotoleune |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081772A (en) * | 2018-08-06 | 2018-12-25 | 江苏焕鑫新材料股份有限公司 | A kind of technique and device effectively improving the chloro- 3,5- xylenol chlorination reaction production efficiency of 4- |
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| CN101456793A (en) * | 2007-12-13 | 2009-06-17 | 长春人造树脂厂股份有限公司 | Method for continuous producing dichlorohydrin and apparatus thereof |
| CN101633601A (en) * | 2008-07-25 | 2010-01-27 | 浙江省东阳市兴华化工有限公司 | Industrial production method for 2, 6-dichlorotoluene |
| CN102285902A (en) * | 2010-06-17 | 2011-12-21 | 刘�文 | Chlorination process method for production tower of para-cyanobenzyl chloride (ortho-cyanobenzyl chloride) |
| CN105367380A (en) * | 2015-12-01 | 2016-03-02 | 南京钟腾化工有限公司 | Method for preparing 2,4-dichlorotoluene by using parachlorotoluene |
| CN205740832U (en) * | 2016-07-05 | 2016-11-30 | 湖北鑫统领万象科技有限公司 | Produce triisopropanolamine, the common apparatus of triethanolamine |
-
2017
- 2017-11-21 CN CN201711166007.0A patent/CN107827703A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456793A (en) * | 2007-12-13 | 2009-06-17 | 长春人造树脂厂股份有限公司 | Method for continuous producing dichlorohydrin and apparatus thereof |
| CN101633601A (en) * | 2008-07-25 | 2010-01-27 | 浙江省东阳市兴华化工有限公司 | Industrial production method for 2, 6-dichlorotoluene |
| CN102285902A (en) * | 2010-06-17 | 2011-12-21 | 刘�文 | Chlorination process method for production tower of para-cyanobenzyl chloride (ortho-cyanobenzyl chloride) |
| CN105367380A (en) * | 2015-12-01 | 2016-03-02 | 南京钟腾化工有限公司 | Method for preparing 2,4-dichlorotoluene by using parachlorotoluene |
| CN205740832U (en) * | 2016-07-05 | 2016-11-30 | 湖北鑫统领万象科技有限公司 | Produce triisopropanolamine, the common apparatus of triethanolamine |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081772A (en) * | 2018-08-06 | 2018-12-25 | 江苏焕鑫新材料股份有限公司 | A kind of technique and device effectively improving the chloro- 3,5- xylenol chlorination reaction production efficiency of 4- |
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Application publication date: 20180323 |