CN202099218U - Device for producing ursol by liquid phase continuous hydrogenation method - Google Patents
Device for producing ursol by liquid phase continuous hydrogenation method Download PDFInfo
- Publication number
- CN202099218U CN202099218U CN2011202220991U CN201120222099U CN202099218U CN 202099218 U CN202099218 U CN 202099218U CN 2011202220991 U CN2011202220991 U CN 2011202220991U CN 201120222099 U CN201120222099 U CN 201120222099U CN 202099218 U CN202099218 U CN 202099218U
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- ursol
- guide shell
- straight tube
- liquid phase
- 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.)
- Expired - Lifetime
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a device for producing ursol by a liquid phase continuous hydrogenation method, which comprises a paranitroaniline storage tank (1), a carbinol storage tank (3), a primary hydrogenation reactor (5), a secondary hydrogenation reactor (8), a discharged liquid control tank (11), catalyst settling tanks (12 and 13) and a fractionating column (14). The primary hydrogenation reactor (5) is serially connected with the secondary hydrogenation reactor (8), the primary hydrogenation reactor (5) is respectively connected with the paranitroaniline storage tank (1) and the carbinol storage tank (3) by the aid of metering pumps (2 and 4) through pipelines, the primary hydrogenation reactor (5) and the secondary hydrogenation reactor (8) are provided with a hydrogen inlet respectively, a discharge outlet of the secondary hydrogenation reactor is communicated with the discharged liquid control tank (11) through a pipeline, the discharged liquid control tank (11) is connected with the catalyst settling tanks (12 and 13) through pipelines, and discharge outlets of the catalyst settling tanks are communicated with the fractionating column (14) through pipelines. The device for producing ursol by the liquid phase continuous hydrogenation method is low in cost, high in yield, fine in safety and is environment-friendly.
Description
Technical field
The utility model relates to the production equipment of Ursol D, and particularly the continuous liquid phase hydrogenation method is produced the device of Ursol D.
Background technology
Ursol D is one of the simplest aromatic diamines; It also is a kind of midbody that is widely used; Can be used for producing azoic dyestuff, high molecular polymer also can be used for producing the fur dyeing agent; Rubber antioxidant and photo development agent, the check iron that Ursol D is still commonly used in addition and the sensitive reagents of copper.Ursol D is very important dyestuff intermediate, is mainly used in aramid fiber, azoic dyestuff, thioxine dyes, matching stain etc.At present the main production of domestic production Ursol D is to be raw material with the p-Nitroaniline, is got by iron powder reducing.The shortcoming of this method is: product yield is low, and total recovery is less than 85%; Environmental pollution is serious, and the iron mud of generation is hard to manage; Operating environment is poor.
The domestic report that also has the shortening method to produce Ursol D, but interrupter method production all adopted, the interrupter method equipment capacity is low, and operation labour intensity is big, need carry out hydrogen exchange to reaction kettle in the production process, and hydrogen consumption is high, poor stability.
Summary of the invention
The purpose of the utility model is: the device that provides a kind of continuous liquid phase hydrogenation method to produce Ursol D, this device have that cost is low, yield is high, security is good and eco-friendly characteristics, solve to have the technical problem that exists in the technology now.
The technical solution of the utility model is: this production equipment comprises p-Nitroaniline storage tank, methyl alcohol storage tank, one-level hydrogenation reaction kettle, secondary hydrogenation reaction kettle, discharging liquid level controlling tank, catalyst sedimentation groove, solvent and rectifying tower; One-level hydrogenation reaction kettle series connection secondary hydrogenation reaction kettle; On the one-level hydrogenation reaction kettle, connect p-Nitroaniline storage tank and methyl alcohol storage tank through pipeline through volume pump respectively; Establish hydrogen inlet on the I and II hydrogenation reaction kettle; The discharge port of secondary hydrogenation reaction kettle is communicated with the out-feed liquid controlling tank through pipeline, and the out-feed liquid controlling tank is communicated with two catalyst sedimentation grooves through pipeline, and the discharge port of catalyst sedimentation groove is communicated with fractionate through pipeline.
Wherein, on the I and II hydrogenation reaction kettle, connect catalyzer through pipeline through ball valve respectively and add jar.
Wherein, The I and II hydrogenation reaction kettle is made up of lower cover, upper cover and straight tube, straight tube weld upper cover, lower cover formation reaction kettle up and down respectively, establish rinse mouth in the bottom of lower cover; In straight tube, guide shell is installed; Annular space between guide shell and the straight tube is installed heat exchange coil, on the barrel of straight tube, establishes entrance of cooling water, cooling water outlet and discharge port, on upper cover, establishes p-Nitroaniline opening for feed, methyl alcohol import, hydrogen inlet, TM mouth, gauge port and catalyzer and adds mouth; Stirring rake is installed through flange in top at upper cover, and the impeller of stirring arm is positioned at guide shell.
Wherein, on upper cover, establish manhole, visor mouth and relief valve port.
Wherein, on lower cover, establish the TM mouth.
Wherein, the sectional area of guide shell is S1, and the net sectional area of the annular space between guide shell and the straight tube is S2, and S2 is 1-1.5 a times of S1.
Wherein, the upper end of guide shell exceeds 5-10cm than the superiors of heat exchange coil, aligns with the orlop of heat exchange coil in the lower end of guide shell, and the lower end of guide shell is not less than the lower surface of straight tube.
Wherein, the diameter of the impeller of the stirring rake in guide shell is the 30-70% of draft tube diameter.
Wherein, be provided with the discharging weir in straight inboard of discharge port one side, the top on discharging weir is airtight, the bottom on discharging weir and reaction kettle internal communication, and the bottom on discharging weir is not less than 1/4th of guide shell height to the distance of guide shell lower end.
Wherein, two flange differential pressure levelmeters are installed on the out-feed liquid controlling tank are measured the liquid level of controlling tank, thereby control the liquid level of secondary hydrogenation still indirectly.
Wherein, The catalyst sedimentation groove is made up of straight tube in top and bottom cone; Lower end side at straight tube is provided with discharge port; As far as possible near the bottom of straight tube, the cone angle of the cone of catalyst sedimentation groove is established the catalyst recovery mouth less than 90 degree in the bottom of cone to discharge port under the prerequisite that satisfies the apparatus processing condition.
The utlity model has following advantage: 1, the nitro of aromatic nitro compound is amino by hydrogen reducing under catalyst action, and temperature, the pressure of reaction are lower, and equipment manufacturing cost is low; 2, adopt methyl alcohol to make solvent, increase the touch opportunity of catalyzer, hydrogen, nitro-compound, solvent low price, in liberal supply; 3, the speed of response according to reduction reaction obtains reaction time, confirms input speed by reaction time, can know from reaction time, and operation of equipment elasticity is big; 4, product yield is high, and in p-Nitroaniline, total recovery is greater than 95%; 5, continuous production, labour intensity is little; 6, cleaner production greatly reduces the environmental pollution of iron powder reducing method; 7, serialization production, the p-Nitroaniline total content is low in the system, has avoided the big shortcoming of material total amount in the interrupter method system, need not carry out repeatedly hydrogen exchange in production process, accomplishes essential safety; 8, two flange differential pressure levelmeters are installed on the out-feed liquid controlling tank and are measured the liquid level of controlling tank, thereby control the liquid level of secondary hydrogenation still indirectly; If the liquid level the during discharging of secondary hydrogenation still is when the lower edge of the half the or discharge port of discharge port; Cause hydrogen entering follow-up system in the still easily; Both caused waste also to have potential safety hazard; When guaranteeing discharging, the liquid level in the secondary hydrogenation still need be carried out liquid level control to secondary hydrogenation still on discharge port; In secondary hydrogenation still; Because the effect of stirring also has a large amount of hydrogen to feed liquid in the still, the liquid level of hydrogenation still is difficult to measure, and the out-feed liquid controlling tank links to each other with secondary hydrogenation still; Liquid level is higher than the pipe connecting between secondary hydrogenation still and the out-feed liquid controlling tank in the still; Like this, the liquid level of out-feed liquid controlling tank is relatively stable, is easy to measure; During discharging, the liquid level of control out-feed liquid controlling tank guarantees that hydrogen can not get into the system of back on the pipe connecting of secondary hydrogenation still and out-feed liquid controlling tank.
Description of drawings
Fig. 1 is the production equipment block diagram of the utility model.
Fig. 2 is the structural representation of hydrogenation reaction kettle.
Fig. 3 is the vertical view of Fig. 2.
Fig. 4 is the structural representation of catalyst sedimentation groove.
Among the figure: 1 p-Nitroaniline storage tank, 2 volume pumps, 3 methyl alcohol storage tanks, 4 volume pumps, 5 one-level hydrogenation reaction kettles, 6 one-level ball valves; 7 one-level catalyzer are added jar, 8 secondary hydrogenation reaction kettles, and 9 secondary ball valves, 10 second catalysts are added jar, 11 out-feed liquid controlling tank, 12 catalyst sedimentation grooves; 13 catalyst sedimentation grooves, 14 fractionates, 15 rinse mouths, 16 lower covers, 17 lower cover TM mouths, 18 guide shells; 19 heat exchange coils, 20 straight tubes, 21 entrance of cooling water, 22 upper covers, 23 p-Nitroaniline opening for feeds; 24 flanges, 25 hydrogen inlets, 26 cooling water outlets, 27 discharge ports, 28 discharging weirs; 29 visor mouths, 30 manholes, 31 methanol feeding mouths, 32 visor mouths, 33 upper cover TM mouths; 34 gauge ports, 35 catalyzer are added mouth, 36 relief valve port, 37 whisking appliances, 38 subsider discharge ports, 39 catalyst recovery mouths.
Embodiment
Below in conjunction with accompanying drawing the utility model is described in further detail.Should be understood that just the utility model is described for example, but not limit the scope of the utility model by any way.Easy in order to narrate, omitted annexes such as the mouth of pipe conventional on valve conventional on the pipeline, the storage tank, manhole, instrumentation tap, bearing in the explanation of the utility model, the those skilled in the art of the industry can design as required.The those of ordinary skill of the industry can be made many modification and improvement, for example changes the charging metering method, and the mouth of pipe of reaction kettle is adjusted, and increases the quantity of reaction kettle, and all these modification, adjustment, improvement all should be regarded as the protection domain of the utility model.
Shown in Fig. 1-4; The production equipment of the utility model comprises p-Nitroaniline storage tank 1, methyl alcohol storage tank 3, one-level hydrogenation reaction kettle 5, secondary hydrogenation reaction kettle 8, out-feed liquid controlling tank 11, catalyst sedimentation groove 12,13 and fractionate 14; One-level hydrogenation reaction kettle 5 series connection secondary hydrogenation reaction kettles 8; On one-level hydrogenation reaction kettle 5, connect p-Nitroaniline storage tank 1 and methyl alcohol storage tank 3 through pipeline through volume pump 2,4 respectively; Establish hydrogen inlet on the I and II hydrogenation reaction kettle 5,8; The discharge port of secondary hydrogenation reaction kettle is communicated with out-feed liquid controlling tank 11 through pipeline, and out-feed liquid controlling tank 11 is communicated with two catalyst sedimentation grooves 12,13 through pipeline, and the discharge port of catalyst sedimentation groove is communicated with fractionate 14 through pipeline.
Wherein, on I and II hydrogenation reaction kettle 5,8 respectively through pipeline through one-level ball valve 6, secondary ring valve 9 connect that the one-level catalyzer add jars 7, second catalyst adds jars 10.
Wherein, The I and II hydrogenation reaction kettle is made up of lower cover 16, upper cover 22 and straight tube 19; Straight tube 19 weld upper cover 22 up and down respectively, lower cover 16 constitutes reaction kettles; Establish rinse mouth 15 in the bottom of lower cover 16, in straight tube 19, guide shell 18 is installed, the annular space between guide shell 18 and the straight tube 19 is installed heat exchange coil 20; On the barrel of straight tube 19, establish entrance of cooling water 21, cooling water outlet 26 and discharge port 27; On upper cover 22, establish p-Nitroaniline opening for feed 23, methyl alcohol import 31, hydrogen inlet 25, TM mouth 33, gauge port 34 and catalyzer and add mouth 35, through flange 24 stirring rakes 37 are installed at the top of upper cover 22, the impeller of stirring arm 37 is positioned at guide shell 18.
Wherein, on upper cover 22, establish manhole 30, visor mouth 29,32 and relief valve port 36.
Wherein, on lower cover 16, establish TM mouth 17.
Wherein, the sectional area of guide shell 18 is S1, and the net sectional area of the annular space between guide shell 18 and the straight tube 19 is S2, and S2 is 1-1.5 a times of S1.
Wherein, the upper end of guide shell 18 exceeds 5-10cm than the superiors of heat exchange coil 20, aligns with the orlop of heat exchange coil 20 in the lower end of guide shell 18, and the lower end of guide shell 18 is not less than the lower surface of straight tube 19.
Wherein, the diameter of the impeller of the stirring rake in guide shell 18 37 is the 30-70% of draft tube diameter.
Wherein, be provided with discharging weir 28 in straight 19 inboard of discharge port 27 1 sides, the top on discharging weir 28 is airtight, the bottom on discharging weir 28 and reaction kettle internal communication, and the bottom on discharging weir 28 is not less than 1/4th of guide shell height to the distance of guide shell 18 lower ends.
Wherein, The catalyst sedimentation groove is made up of straight tube in top and bottom cone; Lower end side at straight tube is provided with subsider discharge port 38; As far as possible near the bottom of straight tube, the cone angle of the cone of catalyst sedimentation groove is established catalyst recovery mouth 39 less than 90 degree in the bottom of cone to subsider discharge port 38 under the prerequisite that satisfies the apparatus processing condition.
Wherein, two flange differential pressure levelmeters are installed on the out-feed liquid controlling tank 11.
Claims (9)
1. the continuous liquid phase hydrogenation method is produced the device of Ursol D; It is characterized in that: this production equipment comprises p-Nitroaniline storage tank (1), methyl alcohol storage tank (3), one-level hydrogenation reaction kettle (5), secondary hydrogenation reaction kettle (8), out-feed liquid controlling tank (11), catalyst sedimentation groove (12,13) and fractionate (14); One-level hydrogenation reaction kettle (5) series connection secondary hydrogenation reaction kettle (8); On one-level hydrogenation reaction kettle (5), connect p-Nitroaniline storage tank (1) and methyl alcohol storage tank (3) through pipeline through volume pump (2,4) respectively; The I and II hydrogenation reaction kettle is established hydrogen inlet on (5,8); The discharge port of secondary hydrogenation reaction kettle is communicated with out-feed liquid controlling tank (11), out-feed liquid controlling tank (11) through two catalyst sedimentation grooves of pipe connection (12,13) through pipeline, and the discharge port of catalyst sedimentation groove is communicated with fractionate (14) through pipeline.
2. continuous liquid phase hydrogenation method according to claim 1 is produced the device of Ursol D; It is characterized in that: wherein, on I and II hydrogenation reaction kettle (5,8), connect the I and II catalyzer through pipeline through I and II ball valve (6,9) respectively and add jar (7,10).
3. continuous liquid phase hydrogenation method according to claim 1 is produced the device of Ursol D; It is characterized in that: wherein; The I and II hydrogenation reaction kettle is made up of lower cover (16), upper cover (22) and straight tube (19); Straight tube (19) weld upper cover (22) up and down respectively, lower cover (16) constitutes reaction kettle; Establish rinse mouth (15) in the bottom of lower cover (16); Guide shell (18) is installed in straight tube (19); Annular space between guide shell (18) and the straight tube (19) is installed heat exchange coil (20), on the barrel of straight tube (19), establishes entrance of cooling water (21), cooling water outlet (26) and discharge port (27), on upper cover (22), establishes p-Nitroaniline opening for feed (23), methyl alcohol import (31), hydrogen inlet (25), upper cover TM mouth (33), gauge port (34) and catalyzer and adds mouthful (35); Stirring rake (37) is installed through flange (24) in top at upper cover (22), and the impeller of stirring arm (37) is positioned at guide shell (18).
4. continuous liquid phase hydrogenation method according to claim 3 is produced the device of Ursol D, it is characterized in that: wherein, on upper cover (22), establish manhole (30), visor mouth (29,32) and relief valve port (36); Wherein, on lower cover (16), set end socket TM mouth (17).
5. continuous liquid phase hydrogenation method according to claim 3 is produced the device of Ursol D; It is characterized in that: wherein; The sectional area of guide shell (18) is S1, and the net sectional area of the annular space between guide shell (18) and the straight tube (19) is S2, and S2 is 1-1.5 a times of S1; Wherein, the upper end of guide shell (18) exceeds 5-10cm than the superiors of heat exchange coil (20), aligns with the orlop of heat exchange coil (20) in the lower end of guide shell (18), and the lower end of guide shell (18) is not less than the lower surface of straight tube (19).
6. continuous liquid phase hydrogenation method according to claim 3 is produced the device of Ursol D, and it is characterized in that: wherein, the diameter of the impeller of the stirring rake (37) in guide shell (18) is the 30-70% of draft tube diameter.
7. continuous liquid phase hydrogenation method according to claim 3 is produced the device of Ursol D; It is characterized in that: wherein; Inboard at the straight tube (19) of discharge port (27) one sides is provided with discharging weir (28); The top on discharging weir (28) is airtight, the bottom of discharging weir (28) and reaction kettle internal communication, and the bottom of discharging weir (28) is not less than 1/4th of guide shell height to the distance of guide shell (18) lower end.
8. continuous liquid phase hydrogenation method according to claim 3 is produced the device of Ursol D; It is characterized in that: wherein; The catalyst sedimentation groove is made up of straight tube in top and bottom cone, is provided with subsider discharge port (38) straight lower end side, and subsider discharge port (38) is tried one's best under the prerequisite that satisfies the apparatus processing condition near the bottom of straight tube; The cone angle of the cone of catalyst sedimentation groove is established catalyst recovery mouth (39) less than 90 degree in the bottom of cone.
9. continuous liquid phase hydrogenation method according to claim 3 is produced the device of Ursol D, it is characterized in that: wherein, out-feed liquid controlling tank (11) goes up the liquid level that two flange differential pressure levelmeter control hydrogenation stills and out-feed liquid controlling tank are installed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202220991U CN202099218U (en) | 2011-06-28 | 2011-06-28 | Device for producing ursol by liquid phase continuous hydrogenation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202220991U CN202099218U (en) | 2011-06-28 | 2011-06-28 | Device for producing ursol by liquid phase continuous hydrogenation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202099218U true CN202099218U (en) | 2012-01-04 |
Family
ID=45385243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202220991U Expired - Lifetime CN202099218U (en) | 2011-06-28 | 2011-06-28 | Device for producing ursol by liquid phase continuous hydrogenation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202099218U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143883A (en) * | 2019-05-28 | 2019-08-20 | 中国神华煤制油化工有限公司 | A kind of process for selective hydrogenation |
| CN110452126A (en) * | 2019-08-16 | 2019-11-15 | 上海鸿源鑫创材料科技有限公司 | Pass through liquid-phase catalyst hydrogenation reduction method in a kind of preparation process of p-phenylenediamine |
-
2011
- 2011-06-28 CN CN2011202220991U patent/CN202099218U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110143883A (en) * | 2019-05-28 | 2019-08-20 | 中国神华煤制油化工有限公司 | A kind of process for selective hydrogenation |
| CN110143883B (en) * | 2019-05-28 | 2023-03-03 | 中国神华煤制油化工有限公司 | Hydrogenation reaction method |
| CN110452126A (en) * | 2019-08-16 | 2019-11-15 | 上海鸿源鑫创材料科技有限公司 | Pass through liquid-phase catalyst hydrogenation reduction method in a kind of preparation process of p-phenylenediamine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101906046B (en) | Method and device for producing o-phenylenediamine by continuous liquid phase hydrogenation | |
| CN102827008B (en) | Method and device for producing phenylenediamine by taking water as solvent through liquid phase continuous hydrogenation method | |
| CN102276479A (en) | Method and device for producing p-phenylenediamine by using liquid phase continuous hydrogenation method | |
| CN102491905B (en) | Method and device for co-production of o-phenylenediamine and p-phenylenediamine | |
| CN202099218U (en) | Device for producing ursol by liquid phase continuous hydrogenation method | |
| CN203021488U (en) | Preparation system of carboxy styrene-butadiene latex | |
| CN202849299U (en) | Reflux device for unsaturated polyester resin reaction kettle | |
| CN101811745A (en) | Treating device for extracting naphthalene sulfonic acid waste liquor | |
| CN210993129U (en) | Increase settler that catalyst subsides | |
| CN204996456U (en) | Horizontal alkylation reaction ware of vibration proof | |
| CN213977502U (en) | Continuous production device of hydroxyl acrylic resin | |
| CN204447954U (en) | A kind of reactor polymerization single polymerization monomer feed arrangement | |
| CN202478916U (en) | Production device for liquid water-soluble resin | |
| CN207973695U (en) | A kind of liquid-phase catalyst hydrogenating reduction method prepares the preparation system of p-phenylenediamine | |
| CN207862267U (en) | A kind of carbon black oil process units | |
| CN210683648U (en) | Continuous polymerization system of C5/C9 copolymerized petroleum resin | |
| CN211896736U (en) | Production device of N-cyanoethyl-N-phenethylaniline | |
| CN205517643U (en) | Reaction unit with inlet pipe under many liquid | |
| CN208136161U (en) | With methanol, the process units of naphtha etherificate chain extension technique light aromatics gasoline | |
| CN203007184U (en) | Reaction sub-system for producing carboxylic styrene butadiene latex | |
| CN203525701U (en) | Reaction tower kettle | |
| CN218475251U (en) | Continuous flow industrialization equipment for producing 2,4 dinitroaniline | |
| CN210065613U (en) | C5 petroleum resin polymerization apparatus for producing | |
| CN214485683U (en) | Four-stage flash evaporation four-stage membrane tower heat absorption system | |
| CN1962607A (en) | Method for synthesizing allylamine using transfer line reactor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20120104 |
|
| CX01 | Expiry of patent term |