CN204638167U - Chlorination processes tower falls outside tower - Google Patents
Chlorination processes tower falls outside tower Download PDFInfo
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- CN204638167U CN204638167U CN201520341420.6U CN201520341420U CN204638167U CN 204638167 U CN204638167 U CN 204638167U CN 201520341420 U CN201520341420 U CN 201520341420U CN 204638167 U CN204638167 U CN 204638167U
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Abstract
The utility model provides outside a kind of tower and falls chlorination processes tower, save group up and down by multiple tower and be connected on one, each tower joint has sky cylinder, tower tray is connected with in empty cylinder lower end, empty cylinder interior has riser and abat-vent, abat-vent cover cap is on riser, and riser enters this tower joint thus for the gas more than needed of lower squarer joint, and the wall of the lower end of abat-vent leaves many Minute pores.The wall of empty cylinder side is provided with inlet, and the liquid keeping supplying squarer joint enters this tower joint; The wall of empty cylinder opposite side has a liquid outlet, and liquid outlet is communicated with the tube connector arranged straight up, and tube connector is communicated with downspout, and this downspout is communicated with the inlet of next tower joint.The middle and upper part of empty cylinder side is provided with Balance Air import, and is communicated with the upper end of tube connector.Chlorination tower of the present utility model has that structure is simple, and maintenance rate is low, and temperature in reaction system and pressure drop can accurately control, and the purity of product is higher.
Description
Technical field
The utility model relates to production equipment and the production technology of trichloroacetaldehyde.
Background technology
Trichloroacetaldehyde (or claiming chloral) is one of halogen derivatives of a kind of important hydroxy compounds, is colourless volatile oily liquids, irritant smell, boiling point 97.8 DEG C, fusing point-57.5 DEG C, relative density 1.5121.Energy water-soluble, ethanol, EC, generate trichloroacetaldehyde hydrate (or claiming fluorocarbon oil) with hydrate.Trichloroacetaldehyde can be widely used in produces agricultural chemicals, medicine and the aspect such as organic synthesis is industrial, its production method has ethanol chloridising and acetaldehyde chloridising, ethanol tower type chlorination method is now mainly adopted to produce in industry, be that raw material reacts with chlorine and water and generates fluorocarbon oil at 80 ~ 90 DEG C with ethanol, again with strong sulfuric acid response, obtain through distillation.
Ethanol chlorination process reaction mechanism is more complicated, side reaction is also more, the material that process exists has chlorine, alcohol, trichloroacetaldehyde, hydrogen chloride, hydrochloric acid, acetic acid, trichloroacetic acid, ethyl trichloroacetate, chloroethanes and hypochlorous acid etc., the most of corrosivity of these materials is very strong, and certain reaction temperature and pressure also increase the corrosivity of material, so require higher to the corrosion resistance of tower, it is main that the material of current reactor is mainly selected nonmetal.
In order to improve production capacity and yield, have employed tower chlorination production trichloroacetaldehyde first in industries in 1977, in during chlorination tower tower joint is saved by riser, abat-vent, tower, downspout, tower tray etc. containing inlet and liquid outlet form, and use more than 30 year till today.Some shortcomings are day by day obvious, as: downspout, riser, abat-vent, tower tray etc. are all adopt ceramic integral sintering to form, complex structure, processing difficulties and of low quality, and yield rate is low, and many producers have been reluctant order, and buying is more and more difficult.But this version also can only adopt ceramic making at present, hinder the use of some economic anticorrosive materials.But due to High Pressure Difference, corrosive operating mode and crudy, pottery is easily cracked, service life was less than 3 years; Ventilation assembly and interior downspout all use resin bonding on tower tray, and after using a period of time, resin can lose efficacy, and causes leakage, causes column plate to lose efficacy, and reduce the rate of output; The feed tube of column plate, drain pipe all with fragility greatly can not load-bearing graphite head bonding with tower tray.All situations are all easy to cause a large amount of Leakage Gas environmental pollution above, Whole Equipment shortening in service life.
The method of number of patent application a kind of continuously synthesizing trichloracetic aldehyde that has been the disclosure of the invention of 2010101217686 and device thereof.Ethanol and chlorine counter current contacting are reacted, and reactor is made up of 3 grades of circulation flow reactors and 1 grade of packed column reactor or plate-type reactor, and the mol ratio of chlorine and ethanol is 3.5 ~ 4.5: 1, and the mol ratio of water and ethanol is 0.6 ~ 1.5: 1.The temperature of the 1st stage reactor is 10 DEG C ~ 30 DEG C, and the temperature of the 2nd stage reactor is 50 DEG C ~ 75 DEG C, and the temperature of 3rd level reactor is 80 DEG C ~ 95 DEG C, and the temperature of the 4th stage reactor is 80 DEG C ~ 110 DEG C.Chlorine by the 2nd grade, 3rd level, the 4th stage reactor bottom pass into, 2nd grade, 3rd level, the 4th stage reactor tail chlorine converge after enter the 1st stage reactor, ethanol is added by the 1st stage reactor, reaction intermediate flows into next stage reactor successively, and water adds respectively at the differing heights of the 4th stage reactor.The temperature subregion of the method is more, controls cumbersome, and the temperature between area postrema is higher than the boiling point of trichloroacetaldehyde, causes part trichloroacetaldehyde to run off.
Number of patent application be 2012104785685 invention relate to a kind of Novel technology for chloral industrial production, belong to chemical production technology field, by the fluorocarbon oil that the chlorination of organic solvent liquid-liquid extraction process process ethanol produces, make it be separated into watery hydrochloric acid aqueous phase and organic phase, organic phase produces high-load trichloroacetaldehyde by rectification process.Do not use the concentrated sulfuric acid as dehydrating agent, thus avoid producing Waste Sulfuric Acid, the yield simultaneously making fluorocarbon oil produce trichloroacetaldehyde reaches more than 97%, and the ethanol in fluorocarbon oil, hemiacetal component are distillated to separate and return to chlorination system, further increase raw material availability.This technique, because consuming organic solvent and more steaminess, brings complicated and steam consumption to increase.
Summary of the invention
Utility model object:
Overcome traditional ethanol chloridising equipment failure rate high, the problem that the rate of output is low, provide a kind of device structure simple, safeguard easily, control flexibly, fall chlorination processes tower outside tower that production cost reduces.
Technical scheme:
Outside tower of the present utility model, chlorination processes tower falls, by multiple tower save group be up and down connected on one (each tower save can have condenser down, the temperature controlling liquid in each tower joint is unlikely to because reaction heat rises so high, cause gas over flood, ensure that the ratio of each reaction composition is suitable), uppermost tower joint top has raw material alcohol entrance, the below of bottom tower joint is that tower reactor (stores fluorocarbon oil, buffering chlorine and water vapour), each tower joint has sky cylinder, (top of empty cylinder and bottom all can with adpting flanges to be connected with tower tray in empty cylinder lower end, be convenient to the connection of upper and lower Ta Jie), empty cylinder interior has riser and abat-vent, abat-vent cover cap is on riser, riser enters this tower joint thus for the gas more than needed of lower squarer joint.Tower tray leaves gross blow hole, as the air inlet of riser.The wall of the lower end of abat-vent leaves many Minute pores.
The wall of empty cylinder side is provided with inlet, and the liquid keeping supplying squarer joint enters this tower joint, the wall of empty cylinder opposite side has a liquid outlet, liquid outlet is communicated with the tube connector arranged straight up, tube connector is provided with and falls liquid outlet, fall liquid outlet downspout and (fall the similar threeway of liquid outlet, the syndeton form that the position of threeway preferably can move up and down along tube connector, to utilize liquid pressure in the equal principle of U-tube two ends sustained height, by regulating the position of the position of threeway and the horizontal pipeline section of downspout, control and adjust the liquid level position in empty cylinder, the time of staying needed for pressure in control tower joint and gas and liquid mixed system react), this downspout is communicated with the inlet of next tower joint (containing one section of feed tube before inlet, downspout and feed tube UNICOM, using the interface equal-height position between tower joint as docking location).
The middle and upper part of empty cylinder side can be provided with Balance Air import, and is communicated with the upper end of tube connector, with the air pressure balance in tube connector in the cylinder that makes to have leisure, and liquid level in make to have leisure liquid level in cylinder and tube connector (namely falling the position that liquid exports to remain basically stable).
The position of inlet is in the middle and lower part of empty cylinder wall surface, and the position of liquid outlet is in the bottom of empty cylinder wall surface.
In the utility model, the position of inlet, a little more than the position of Minute pores, ensures that gas-liquid fully mixes contact; The position of inlet is lower than Balance Air import, and substantially can ensure that Balance Air import is at ullage, inlet is below liquid level.
The position of liquid outlet, lower than the position of Minute pores highest order, ensures that gas has the more sufficient haptoreaction time with also body, ensures that liquid heavier in empty cylinder (be mainly fluorocarbon oil, instead of lighter methyl alcohol and hydrochloric acid) flows out thus.
The mode that abat-vent and tower tray, riser and gross blow hole preferably adopt screw thread or be welded to connect, is convenient to manufacture and install.
Tower tray, riser and abat-vent preferably use commaterial, preferred PTFE material.
Empty cylinder preferably adopts steel lining anti-corrosion material to make, and inlet and liquid outlet are owing to being arranged on the empty cylinder of steel lining anti-corrosion material, and connect more reliable, seal is better.
Run parameter:
In the utility model each tower joint from bottom to top empty cylinder in the temperature range 80-100 DEG C of liquid, ensure that the reaction temperature of fluorocarbon oil is suitable, be no more than the boiling point of chloral and too much useful component is overflowed, ensure the quality of products and become to clear productive rate.Bottom temperature is the highest (regulates the temperature of tower reactor Raw by the pressure and temperature adjusting steam, and by condenser regulates liquid temperature), topmost temperature is minimum, ensure unreacted completely chlorine rise step by step participate in reaction, after arriving tower joint above, chlorine does not run off again a lot from abhiseca, the utilization rate of raw material improves, and the efficiency of reaction system improves.
The air pressure (or claiming the pressure drop of tower joint) of the ullage space of each empty cylinder is the preferred 5Kpa of 3-8Kpa().
Workflow:
Liquid process is fallen in tower: the material of upper strata Ta Jie enters lower floor's tower joint by inlet, together with liquid storage in saving with this tower flows to, save with lower floor tower the gas risen to contact mixing and react, liquid level in empty cylinder is along with reaction rising, when liquid level is parallel with falling liquid exit position, material enters tube connector from liquid outlet, gas phase portion returns sky cylinder interior by Balance Air import, liquid phase part flows into descending trays (liquid phase that undermost tower throttling goes out flow directly into tower reactor after, enter fluorocarbon oil storage tank) by downspout.
Gas process is risen: the chlorine of lower floor's tower joint (or from tower reactor) and light component (alcohol in tower, hydrogen chloride, chloroethanes, methyl alcohol and water vapour) etc. gas entered by the gross blow hole of upper strata Ta Jie and riser, then sky cylinder is entered from many Minute pores of abat-vent, mix with the liquid in this tower joint dish, there is gas liquid reaction and separation process, unreacted chlorine and part light component enter the ullage of sky cylinder, then (gas of the superiors towers joint flows out from tower overhead gas outlet to enter the riser of upper strata Ta Jie, the inlet of this tower joint can be back to) after the condensation of drainer.
Advantage of the present utility model:
Owing to falling the shortcoming of chlorination processes tower in overcoming, adopt the method for falling liquid outside tower, make chlorination tower have structure simple, the features such as easily manufactured, reliability is high, and maintenance rate is low.
And temperature in reaction system, air pressure and pressure drop can accurately control and regulate, and make the purity of product higher.
Feedstock circulation uses, and raw material is not wasted substantially, and finished product yield is higher, does not substantially have three-waste pollution environment.
The utility model can on a large scale in the suitability for industrialized production streamline of trichloroacetaldehyde.
Accompanying drawing explanation
Fig. 1 is the structural representation that tower joint of the present utility model amplifies;
Fig. 2 is overall structure schematic diagram of the present utility model.
In figure, 1-gross blow hole; 2-tower tray; 3-inlet; 4-feed tube; 5-Minute pores; 6-riser; 7-abat-vent; 8-flange; The empty cylinder interior of 9-; The import of 10-Balance Air; 11-downspout; 12-tube connector; 13-liquid outlet; Liquid outlet falls in 14-; 21-alcohol entrance; 22-tower overhead gas exports; 23-drainer.
Detailed description of the invention
Outside tower as shown in Figure 1 and Figure 2, chlorination processes tower falls, save group up and down by multiple tower and be connected on one, uppermost tower joint top has raw material alcohol entrance, each tower joint has sky cylinder, tower tray is connected with in empty cylinder lower end, empty cylinder interior has riser and abat-vent, and abat-vent cover cap is on riser, and riser enters this tower joint thus for the gas more than needed of lower squarer joint; Tower tray leaves gross blow hole, as the air inlet of riser; The wall of the lower end of abat-vent leaves many Minute pores;
The wall of empty cylinder side is provided with inlet, and the liquid keeping supplying squarer joint enters this tower joint; The wall of empty cylinder opposite side has a liquid outlet, and liquid outlet is communicated with the tube connector arranged straight up, and tube connector is provided with and falls liquid outlet, fall liquid outlet downspout, this downspout is communicated with the inlet of next tower joint.
The middle and upper part of empty cylinder side is provided with Balance Air import, and is communicated with the upper end of tube connector, and with the air pressure balance in tube connector in the cylinder that makes to have leisure, the position of inlet is in the middle and lower part of empty cylinder wall surface, and the position of liquid outlet is in the bottom of empty cylinder wall surface.
The position of inlet is a little more than the position of Minute pores, and the position of inlet is lower than Balance Air import.The position of liquid outlet is lower than the position of Minute pores highest order.
Empty cylinder adopts steel lining anti-corrosion material to make, and inlet and liquid outlet are arranged on sky cylinder.
When this equipment runs, control the temperature range 80-95 DEG C of liquid in the empty cylinder of each tower joint, the air pressure of the ullage space of each empty cylinder is 5-8Kpa.
Claims (7)
1. outside a tower, chlorination processes tower falls, save group up and down by multiple tower and be connected on one, uppermost tower joint top has raw material alcohol entrance, the below of bottom tower joint is tower reactor, each tower joint has sky cylinder, is connected with tower tray, it is characterized in that: empty cylinder interior has riser and abat-vent in empty cylinder lower end, abat-vent cover cap is on riser, and riser enters this tower joint thus for the gas more than needed of lower squarer joint; Tower tray leaves gross blow hole, as the air inlet of riser; The wall of the lower end of abat-vent leaves many Minute pores;
The wall of empty cylinder side is provided with inlet, and the wall of empty cylinder opposite side has a liquid outlet, and liquid outlet is communicated with the tube connector arranged straight up, and tube connector is provided with and falls liquid outlet, fall liquid outlet downspout, this downspout is communicated with the inlet of next tower joint.
2. fall chlorination processes tower outside tower as claimed in claim 1, it is characterized in that: fall liquid outlet for moveable three-way connection structure.
3. fall chlorination processes tower outside tower as claimed in claim 1, it is characterized in that: the middle and upper part of empty cylinder side is provided with Balance Air import, and is communicated with the upper end of tube connector; The position of inlet is in the middle and lower part of empty cylinder wall surface, and the position of liquid outlet is in the bottom of empty cylinder wall surface.
4. fall chlorination processes tower outside tower as claimed in claim 1, it is characterized in that: the position of inlet is a little more than the position of Minute pores, and the position of inlet is lower than Balance Air import.
5. fall chlorination processes tower outside tower as claimed in claim 1, it is characterized in that: the position of liquid outlet is lower than the position of Minute pores highest order.
6. fall chlorination processes tower outside tower as claimed in claim 1, it is characterized in that: tower tray, riser and abat-vent use same PTFE material to make.
7. fall chlorination processes tower outside tower as claimed in claim 1, it is characterized in that: inlet and liquid outlet are arranged on sky cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520341420.6U CN204638167U (en) | 2015-05-25 | 2015-05-25 | Chlorination processes tower falls outside tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520341420.6U CN204638167U (en) | 2015-05-25 | 2015-05-25 | Chlorination processes tower falls outside tower |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204638167U true CN204638167U (en) | 2015-09-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520341420.6U Withdrawn - After Issue CN204638167U (en) | 2015-05-25 | 2015-05-25 | Chlorination processes tower falls outside tower |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204638167U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104841341A (en) * | 2015-05-25 | 2015-08-19 | 南通江山农药化工股份有限公司 | Outer-tower downcomer chlorination tower and running process thereof |
-
2015
- 2015-05-25 CN CN201520341420.6U patent/CN204638167U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104841341A (en) * | 2015-05-25 | 2015-08-19 | 南通江山农药化工股份有限公司 | Outer-tower downcomer chlorination tower and running process thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20150916 Effective date of abandoning: 20171114 |
|
| AV01 | Patent right actively abandoned |