CN201610417U - Chlorination reaction device for chloroactic acid production - Google Patents
Chlorination reaction device for chloroactic acid production Download PDFInfo
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- CN201610417U CN201610417U CN2009202909282U CN200920290928U CN201610417U CN 201610417 U CN201610417 U CN 201610417U CN 2009202909282 U CN2009202909282 U CN 2009202909282U CN 200920290928 U CN200920290928 U CN 200920290928U CN 201610417 U CN201610417 U CN 201610417U
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Abstract
The utility model discloses a chlorination reaction device for chloroactic acid production, which comprises a reaction kettle and a condensing system. The condensing system comprises a primary condenser, a secondary condenser and a tertiary condenser which are sequentially connected in series, and a primary buffer tank, a secondary buffer tank and a tertiary buffer tank which are respectively communicated with outlets of the condensers; an outlet of the reaction kettle is communicated with an inlet of the primary condenser; and outlets of the buffer tanks are respectively communicated with the reaction kettle through a primary return pipeline, a secondary primary return pipeline and a tertiary return pipeline. By arranging the three condensers, changing the cooling medium of the condensers and adjusting the processing parameter to perform adaptive adjusting on quantity of reflux, the device improves the main content of chlorinating semi-finished products, reduces the contents of main additional products, such as dichloro acetic acid, trichloroacetic acid and the like, and reduces the chlorination reaction period for chloroactic acid production.
Description
Technical field
The utility model relates to the chemical industry equipment field, relates in particular to a kind of chlorination reaction device of production of chloroacetic acid.
Background technology
Mono Chloro Acetic Acid is an important organic acid, owing in the molecule two important functional groups are arranged, the raw material and the intermediate that can be used as organic synthesis, therefore, Application Areas constantly enlarged in recent years, be widely used in industries such as agricultural chemicals, medicine, dyestuff, oil field chemical, papermaking chemical product, textile auxiliary agent, tensio-active agent, plating and spices and essence, become important organochlorine product.
The acetic acid catalysis chlorination process is to produce chloroacetic main method at present both at home and abroad.It can be divided into two kinds of batch production technology and continuous production technologies again.Batch production technology comprises production stages such as logical chlorinated with chlorine, crystallization kettle intercrystalline, Mono Chloro Acetic Acid separation, wherein chloride process generally is catalyzer with the SULPHUR POWDER, control its consumption and be about acetate 3% of the total amount (mass percent) that feeds intake, be reflected at 90 ℃ of logical chlorine down, control reaction temperature is 96-100 ℃, extract feed liquid every half an hour or one hour and draw an analogy heavily, regulate logical chlorine dose and determine reaction end according to ratio tuple that records and variation tendency.This method is because production technique is fairly simple, institute thinks that most of manufacturer adopts, but this method is owing to reasons such as the restriction of production unit and technology controlling and process, the main at present power consumption height that exists, yield poorly, by-products content such as dichloro acetic acid, trichoroacetic acid(TCA) causes end product quality poor than problems such as height in the work in-process.Therefore at these problems, by research, chlorination reaction device is improved to adapt to chloroacetic chlorination reaction better, to cut down the consumption of energy reaction mechanism and technological principle, improve the quality of products, chloroacetic production is had important economic implications and realistic meaning.
Summary of the invention
Technical problem to be solved in the utility model provides a kind of chlorination reaction device of production of chloroacetic acid, to improve acetic acid conversion, shortens reaction time, cuts down the consumption of energy, and improves product master content.
For solving the problems of the technologies described above, the technical solution of the utility model is:
The chlorination reaction device of production of chloroacetic acid, comprise reactor and condenser system, described condenser system comprises placed in-line successively first-stage condenser, secondary condenser and three grades of condensers, with first-level buffer jar, level 2 buffering jar and three grades of surge tanks of being communicated with respectively with described each condensator outlet, described reactor outlet is communicated with described first-stage condenser import, and the outlet of described each surge tank is communicated with described reactor by one-level return line, secondary return line and three grades of return lines respectively.
Be respectively equipped with gas-liquid separator between described each condenser and each surge tank.
Described one-level return line, secondary return line and three grades of return lines are respectively equipped with under meter.
Owing to adopted technique scheme, the beneficial effects of the utility model are:
1, condenser system of the present utility model is provided with three grades of condensers, and by using different heat-eliminating medium and condensing temperature period in differential responses, different resultant of reaction is carried out condensation respectively recycle.
2, condenser system of the present utility model is provided with three surge tanks, and on three grades of return lines, be respectively equipped with under meter, can control the quantity of reflux in each stage of reaction respectively, mainly rest on the main reaction stage with the control reaction, reduced the generation of side reactions such as dichloro-, three chloros, many chloros, reduced main content of by-products such as dichloro acetic acid, trichoroacetic acid(TCA), thereby improved chlorination work in-process master content, shorten reaction time, also reduced chlorine consumption, reduced production cost.
3, the utility model is by the coolant temperature of control condensers at different levels, light constituents such as active ingredient Acetyl Chloride 98Min., chloro-acetyl chloride have been isolated, reduced the content of light constituent in work in-process and the finished product, improved the main content of the finished product, and isolated light constituent can also recycle or utilized after special processing.
4, the utility model not only can be controlled reaction and mainly rest on the main reaction stage by the backflow of control differential responses resultant, has improved acetic acid conversion, has shortened reaction time, and has improved the accuracy of the adjusting and the judgement of reaction end.
Description of drawings
Accompanying drawing is the synoptic diagram of the utility model embodiment.
Among the figure, 1. reactor; 2. first-stage condenser; 3. secondary condenser; 4. three grades of condensers; 5. first-level buffer jar; 6, level 2 buffering jar; 7. three grades of surge tanks; 8. one-level return line; 9. secondary return line; 10. three grades of return lines; 11. gas-liquid separator; 12. under meter.
Embodiment
As shown in drawings, the chlorination reaction device of production of chloroacetic acid, comprise reactor 1 and condenser system, described condenser system comprises placed in-line successively first-stage condenser 2, secondary condenser 3 and three grades of condensers 4, with the first-level buffer jar 5 that is communicated with respectively with described each condensator outlet, level 2 buffering jar 6 and three grades of surge tanks 7, described reactor 1 outlet is communicated with described first-stage condenser 2 imports, and the outlet of each described surge tank is respectively by one-level return line 8, secondary return line 9 and three grades of return lines 10 are communicated with described reactor 1, in one-level, be respectively equipped with under meter 12 on secondary and three grades of return lines, between described each condenser and each surge tank, be respectively equipped with gas-liquid separator 11.
During the utility model work, use the steam heating material after in reactor 1, dropping into quantitative catalyzer sulphur and acetate, feed chlorinated with chlorine after temperature of charge is heated to 70 ℃ in the reactor 1, heat-eliminating medium in three grades of condensers all uses-10 ℃ chilled brine, gases such as the low-boiling-point substance Acetyl Chloride 98Min. that this moment, reaction generated, chloro-acetyl chloride are condensed, the under meter 12 of three grades of return lines is all opened, and makes whole reactors 1 that reflux back such as Acetyl Chloride 98Min., chloro-acetyl chloride participate in reaction.Carrying out along with reaction, when temperature of charge is increased to 98 ℃ of left and right sides gradually in the reactor 1, increase logical chlorine dose, and with the cooling medium replacement of first-stage condenser 2 is that temperature is the water coolant about 30 ℃, the cooling medium replacement of secondary condenser 3 is 0 ℃ a chilled brine, and the heat-eliminating medium of three grades of condensers 4 still uses-10 ℃ chilled brine.This moment, the liquid under the one-level condensing reflux mainly contained active ingredient chloro-acetyl chloride and raw acetic acid, liquid under B-grade condensation refluxes mainly contains active ingredient Acetyl Chloride 98Min. and chloro-acetyl chloride and raw acetic acid, and the liquid under three grades of condensing refluxes is mainly the active ingredient Acetyl Chloride 98Min..When material ratio in the reactor 1 weighs 1.21-1.24 (80 ℃), close the under meter on one-level return line 8 and the secondary return line 9, the fluid storage that the firsts and seconds condenser condenses is refluxed is in first-level buffer jar 5 and level 2 buffering jar 6, and the quantity of reflux of regulating three grades of return lines 10 is a desired value; After material in reactor proportion reaches 1.30 (80 ℃), the under meter on three grades of return lines is all opened, participate in reaction in the whole reactors 1 that reflux back of various condensed fluids; When material ratio in the reactor 1 weighs 1.34 (80 ℃), the expression reaction is near terminal point, this moment is with the under meter Close All on three grades of return lines, and turn logical chlorine dose down, continue reaction, control reaction mainly rests on a chlorination stage, strengthens and draws an analogy heavy frequency, when proportion stops logical chlorine dose sampling analysis 1.355 the time about.If content is not up to standard, continue insulation, but obstructed chlorine is opened one-level backflow continuation priming reaction a little, up to standard up to content.
Claims (3)
1. the chlorination reaction device of production of chloroacetic acid, comprise reactor and condenser system, it is characterized in that: described condenser system comprises placed in-line successively first-stage condenser, secondary condenser and three grades of condensers, with first-level buffer jar, level 2 buffering jar and three grades of surge tanks of being communicated with respectively with described each condensator outlet, described reactor outlet is communicated with described first-stage condenser import, and the outlet of described each surge tank is communicated with described reactor by one-level return line, secondary return line and three grades of return lines respectively.
2. the chlorination reaction device of production of chloroacetic acid as claimed in claim 1 is characterized in that: be respectively equipped with gas-liquid separator between described each condenser and each surge tank.
3. the chlorination reaction device of production of chloroacetic acid as claimed in claim 1 or 2, it is characterized in that: described one-level return line, secondary return line and three grades of return lines are respectively equipped with under meter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202909282U CN201610417U (en) | 2009-12-25 | 2009-12-25 | Chlorination reaction device for chloroactic acid production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202909282U CN201610417U (en) | 2009-12-25 | 2009-12-25 | Chlorination reaction device for chloroactic acid production |
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| CN201610417U true CN201610417U (en) | 2010-10-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009202909282U Expired - Fee Related CN201610417U (en) | 2009-12-25 | 2009-12-25 | Chlorination reaction device for chloroactic acid production |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102278868A (en) * | 2011-08-02 | 2011-12-14 | 济南圣泉集团股份有限公司 | Exhaust gas recycling technology and device in isothiocyanate preparation |
| CN103386286A (en) * | 2013-07-01 | 2013-11-13 | 安徽省旌德县天益医药化工厂 | Recyclable reaction vessel system |
| CN106220491A (en) * | 2016-07-29 | 2016-12-14 | 河北科技大学 | Production of chloroacetic acid method |
| CN106242961A (en) * | 2016-07-29 | 2016-12-21 | 河北科技大学 | Production of chloroacetic acid equipment |
| CN106669564A (en) * | 2017-03-21 | 2017-05-17 | 河北东华舰化工有限公司 | Emergency treatment system for chloroacetic acid reaction kettle accidents |
| CN108602746A (en) * | 2016-02-04 | 2018-09-28 | Pcc慕卡有限公司 | The method of industrial production chloroacetic acid |
| CN110508092A (en) * | 2019-09-27 | 2019-11-29 | 唐山三友氯碱有限责任公司 | Tai gas of rectifying processing system and its automatic running pattern in production of vinyl chloride by calcium carbide method production technology |
| CN116983701A (en) * | 2023-08-30 | 2023-11-03 | 福建德尔科技股份有限公司 | Rectification control system for preparing trifluoromethane and control method thereof |
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2009
- 2009-12-25 CN CN2009202909282U patent/CN201610417U/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102278868A (en) * | 2011-08-02 | 2011-12-14 | 济南圣泉集团股份有限公司 | Exhaust gas recycling technology and device in isothiocyanate preparation |
| CN103386286A (en) * | 2013-07-01 | 2013-11-13 | 安徽省旌德县天益医药化工厂 | Recyclable reaction vessel system |
| CN108602746A (en) * | 2016-02-04 | 2018-09-28 | Pcc慕卡有限公司 | The method of industrial production chloroacetic acid |
| CN108602746B (en) * | 2016-02-04 | 2022-02-22 | Pcc Mcaa 有限公司 | Method for industrial production of monochloroacetic acid |
| CN106242961A (en) * | 2016-07-29 | 2016-12-21 | 河北科技大学 | Production of chloroacetic acid equipment |
| CN106242961B (en) * | 2016-07-29 | 2018-10-19 | 河北科技大学 | Production of chloroacetic acid equipment |
| CN106220491B (en) * | 2016-07-29 | 2018-12-11 | 河北科技大学 | Production of chloroacetic acid method |
| CN106220491A (en) * | 2016-07-29 | 2016-12-14 | 河北科技大学 | Production of chloroacetic acid method |
| CN106669564B (en) * | 2017-03-21 | 2018-09-28 | 河北东华舰化工有限公司 | A kind of chloroacetate reaction kettle system of accident disposal |
| CN106669564A (en) * | 2017-03-21 | 2017-05-17 | 河北东华舰化工有限公司 | Emergency treatment system for chloroacetic acid reaction kettle accidents |
| CN110508092A (en) * | 2019-09-27 | 2019-11-29 | 唐山三友氯碱有限责任公司 | Tai gas of rectifying processing system and its automatic running pattern in production of vinyl chloride by calcium carbide method production technology |
| CN110508092B (en) * | 2019-09-27 | 2021-05-28 | 唐山三友氯碱有限责任公司 | Rectification tail gas treatment system in calcium carbide method chloroethylene production process and automatic operation mode thereof |
| CN116983701A (en) * | 2023-08-30 | 2023-11-03 | 福建德尔科技股份有限公司 | Rectification control system for preparing trifluoromethane and control method thereof |
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Granted publication date: 20101020 Termination date: 20111225 |