CN104174348B - Neutralization reaction kettle and neutralization reaction method - Google Patents
Neutralization reaction kettle and neutralization reaction method Download PDFInfo
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- CN104174348B CN104174348B CN201310187925.7A CN201310187925A CN104174348B CN 104174348 B CN104174348 B CN 104174348B CN 201310187925 A CN201310187925 A CN 201310187925A CN 104174348 B CN104174348 B CN 104174348B
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- caustic soda
- liquid caustic
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Abstract
The present invention relates to fixed reactor field, it is therefore an objective to provides a kind of neutralization reaction kettle and neutralization reaction method.A kind of neutralization reaction kettle, if including kettle, the gusset main shaft being pivotally connected provided with dried layer agitating paddle and with kettle and the motor for being fixedly connected and being connected with spindle drive with kettle；Described neutralization reaction kettle also includes liquid caustic soda pipe, pipeline swivel joint, liquid caustic soda delivery pump and heater；The gusset of main shaft is provided with several jet pipes；Main shaft is provided with the mesopore connected with lower surface insertion and with jet pipe；The lower end of main shaft is connected by pipeline swivel joint with one end of liquid caustic soda pipe；The other end of liquid caustic soda pipe stretches out the bottom of kettle and the outlet of liquid caustic soda delivery pump；Liquid caustic soda pipe is fixedly connected with kettle；The top of kettle is provided with charge door；The bottom of kettle is provided with drain hole.Thoroughly, product residue acid number is low, and liquid caustic soda consumption is small for the neutralization reaction kettle neutralization reaction.
Description
Technical field
The present invention relates to fixed reactor field, especially a kind of neutralization reaction kettle and neutralization reaction method.
Background technology
Esterification, neutralization reaction and washed reaction are the important steps in environment-friendlyplasticizer plasticizer production process, and esterification is anti-
Answer, neutralization reaction and washed reaction are generally carried out in reactor；Chinese patent notification number CN 102580658A disclosure of the invention
A kind of stirred autoclave, mainly including the agitating device in reaction kettle body, reaction kettle body, the charging aperture on reaction kettle body top and
There are one or more drain pipes on the discharging opening of reaction kettle body bottom, reactor body sidewall, drain pipe one end is located at reaction kettle body
Interior, the other end is provided with Drainage pipe through reactor body sidewall and after being provided with valve, valve.Esterification obtain to benzene
The a small amount of terephthalic acid (TPA) that reaction is not remained completely contained in diformazan dioctyl phthalate crude product, neutralization reaction is certain by adding
The liquid caustic soda of amount and the terephthalic acid (TPA) of residual carry out neutralization reaction, obtain product DOTP；And by terephthaldehyde
Dioctyl phthalate, para-phthalic sodium and water stratification；Neutralization reaction is carried out with traditional stirred autoclave, there is neutralization reaction
Not thoroughly, product residue acid number is high, the big deficiency of liquid caustic soda consumption；Therefore, a kind of neutralization reaction is designed thoroughly, product residue acid
It is worth low, the small neutralization reaction kettle of liquid caustic soda consumption and neutralization reaction method, as urgent problem to be solved.
The content of the invention
The invention aims to overcome to carry out neutralization reaction with traditional stirred autoclave at present, there is neutralization reaction
Not thoroughly, product residue acid number is high, and there is provided a kind of neutralization reaction thoroughly, product residue acid number is low for the big deficiency of liquid caustic soda consumption,
The small neutralization reaction kettle of liquid caustic soda consumption and neutralization reaction method.
The present invention concrete technical scheme be：
A kind of neutralization reaction kettle, if including kettle, gusset provided with dried layer agitating paddle and with kettle be pivotally connected main shaft and and kettle
The motor that body is fixedly connected and is connected with spindle drive；Described neutralization reaction kettle also includes liquid caustic soda pipe, pipeline swivel joint, liquid
Alkali delivery pump and heater；The gusset of main shaft is provided with several jet pipes；Main shaft is provided with and lower surface insertion and connected with jet pipe
Mesopore；The lower end of main shaft is connected by pipeline swivel joint with one end of liquid caustic soda pipe；The other end of liquid caustic soda pipe stretches out kettle
Bottom and the outlet of liquid caustic soda delivery pump；Liquid caustic soda pipe is fixedly connected with kettle；The top of kettle is provided with charge door；The bottom of kettle
Portion is provided with drain hole.Thoroughly, product residue acid number is low, and liquid caustic soda consumption is small for the neutralization reaction kettle neutralization reaction.
Preferably, several described jet pipes are located at the most downside of last layer agitating paddle and radially equal along the gusset of main shaft
Cloth；The upside of each jet pipe gusset is provided with least one liquid caustic soda nozzle.Jet pipe rotates with the rotation of agitating paddle, sprays more equal
It is even；The density ratio plasticizer density of liquid caustic soda is high, and liquid caustic soda sprays upwards progressively to be moved down when carrying out neutralization reaction, with terephthalic acid (TPA)
Dioctyl ester crude product is mixed and reaction time lengthening effect is more preferable.
Preferably, described heater include hotline heater, be wrapped on the outside of kettle gusset and with kettle
Side heat pipe that gusset is fixedly connected and the bottom heat pipe being fixedly connected with the bottom surface of kettle；The two ends of hotline heater respectively with side
One end of heat pipe and one end connection of bottom heat pipe；The other end of side heat pipe is connected with the other end of bottom heat pipe.Heater is simple
It is practical.
Preferably, described bottom heat pipe include outer race tube, inner ring pipe and several be uniformly distributed along the circumference and respectively with outer ring
Manage the radial direction connecting leg connected with inner ring pipe.Have the effect of the intensity of heating and enhancing kettle bottom surface concurrently.
Preferably, described side heat pipe is semi-circular tube；Bottom heat pipe is semi-circular tube.Heating effect is good.
Preferably, described liquid caustic soda delivery pump is measuring pump.Measuring pump is one kind of reciprocating pump, can adjust control
Flow.
The neutralization reaction method of described neutralization reaction kettle, it is characterized in that：（1）The DOTP of specified quantity
Crude product is added in kettle from charge door；（2）Open motor and drive agitating paddle stirring DOTP crude product；（3）Stirring
Mix in the state of oar stirring and jet pipe rotation, open hotline heater, conduction oil is by side heat pipe and bottom heat pipe in kettle
DOTP crude product heat temperature raising；（4）Liquid caustic soda delivery pump is opened, liquid caustic soda is under liquid caustic soda conveying pumping action through mesopore
Spray to enter from jet pipe and mixed in kettle with DOTP crude product, until reaching and DOTP crude product
Regulation proportioning；（5）When the mixed liquid temperature degree of DOTP crude product and liquid caustic soda reaches 110 DEG C, isothermal reaction is kept, directly
Reaction end, and stratification are reached to neutralization reaction；（6）By drain hole by DOTP, terephthalic acid (TPA)
Sodium and water stratification are released.
Neutralization reaction method makes liquid caustic soda be progressively uniformly added into and DOTP crude product with the rotation of agitating paddle
Mix and react, the time for reaching reaction end can be shortened and liquid caustic soda consumption is small.
Compared with prior art, the beneficial effects of the invention are as follows：The one, neutralization reaction kettle neutralization reactions are thorough, and product is residual
Stay acid number low, liquid caustic soda consumption is small.Two, jet pipes rotate with the rotation of agitating paddle, spray more uniform；The density ratio plasticising of liquid caustic soda
Agent density is high, and liquid caustic soda sprays upwards progressively to be moved down when carrying out neutralization reaction, is mixed with DOTP crude product and anti-
Effect is lengthened between seasonable more preferable.Three, heaters are simple and practical.Four, bottoms heat pipes include outer race tube, inner ring pipe and radial direction connecting leg,
Have the effect of the intensity of heating and enhancing kettle bottom surface concurrently.Five, sides heat pipes and bottom heat pipe are semi-circular tube, and heating effect is good.Six,
Measuring pump is one kind of reciprocating pump, can adjust control flow.Seven, neutralization reaction methods make liquid caustic soda with the rotation of agitating paddle
Turn progressively to be uniformly added into mix and react with DOTP crude product, the time for reaching reaction end and liquid can be shortened
Quantity of alkali consumption is small.
Brief description of the drawings
Fig. 1 is a kind of structural representation of the present invention；
Fig. 2 is Fig. 1 A direction views.
In figure：Liquid caustic soda pipe -1, pipeline swivel joint -2, kettle -3, charge door -31, drain hole -32, main shaft -4, stirring
Oar -41, mesopore -42, jet pipe -5, liquid caustic soda nozzle -51, hotline heater -6, side heat pipe -7, bottom heat pipe -8, outer race tube -81,
Inner ring pipe -82, radial direction connecting leg -83, liquid caustic soda delivery pump -9, motor -10, decelerator -11, shaft coupling -12.
Embodiment
It is shown below in conjunction with the accompanying drawings that the present invention is described further.
As shown in accompanying drawing 1, accompanying drawing 2：A kind of neutralization reaction kettle, including kettle 3, gusset have three layers of agitating paddle 41 and and kettle
Body 3 is connected by the main shaft 4 of bearing hinge joint and with the mode connects for screw of kettle 3 and by decelerator 11 and the transmission of shaft coupling 12 with main shaft 4
Motor 10, liquid caustic soda pipe 1, pipeline swivel joint 2, liquid caustic soda delivery pump and the heater connect；The gusset of main shaft 4 has four jet pipes
5；The mesopore 42 that main shaft 4 has with lower surface insertion and connected with jet pipe 5；The lower end of main shaft 4 passes through pipeline swivel joint 2 and liquid
One end connection of alkali pipe 1；The other end of liquid caustic soda pipe 1 stretches out the bottom of kettle 3 and the outlet of liquid caustic soda delivery pump 9；Liquid caustic soda pipe 1
Welded with kettle 3；The top of kettle 3 has charge door 31；The bottom of kettle 3 has drain hole 32.
Four described jet pipes 5 are located at the most downside of last layer agitating paddle 41 and along the gusset radial equipartition of main shaft 4；Each
The upside of the gusset of jet pipe 5 has two liquid caustic soda nozzles 51.
Described heater includes hotline heater 6, is wrapped on the outside of the gusset of kettle 3 and welded with the gusset of kettle 3
The side heat pipe 7 connect and the bottom heat pipe 8 with the bottom surface welding of kettle 3；The two ends of hotline heater 6 respectively with side heat pipe 7 one
End and one end of bottom heat pipe 8 are connected；The other end of side heat pipe 7 is connected with the other end of bottom heat pipe 8.
Described bottom heat pipe 8 include outer race tube 81, inner ring pipe 82 and six be uniformly distributed along the circumference and respectively with outer race tube 81 and
The radial direction connecting leg 83 that inner ring pipe 82 is connected.
Described side heat pipe 7 is semi-circular tube；Bottom heat pipe 8 is semi-circular tube.
Described liquid caustic soda delivery pump 9 is measuring pump.
The neutralization reaction method of described neutralization reaction kettle, it is characterized in that：（1）The DOTP of specified quantity
Crude product is added in kettle 3 from charge door 31；（2）Open motor 10 and drive the stirring DOTP crude product of agitating paddle 41；
（3）In the state of the stirring of agitating paddle 41 and jet pipe 5 are rotated, hotline heater 6 is opened, conduction oil passes through side heat pipe and bottom heat
Pipe is to the DOTP crude product heat temperature raising in kettle 3；（4）Liquid caustic soda delivery pump 9 is opened, liquid caustic soda is in liquid caustic soda delivery pump
9 effect under through mesopore 42 from jet pipe 5 spray enter kettle 3 in mixed with DOTP crude product, up to reach with it is right
The regulation proportioning of dioctyl phthalate crude product；（5）The mixed liquid temperature degree of DOTP crude product and liquid caustic soda reaches 110 DEG C
When, isothermal reaction is kept, until neutralization reaction reaches reaction end, and stratification；（6）By drain hole 32 by terephthaldehyde
Dioctyl phthalate, para-phthalic sodium and water stratification are released.
The beneficial effects of the invention are as follows：Thoroughly, product residue acid number is low, liquid caustic soda consumption for the neutralization reaction kettle neutralization reaction
It is small.Jet pipe rotates with the rotation of agitating paddle, sprays more uniform；The density ratio plasticizer density of liquid caustic soda is high, and liquid caustic soda sprays upwards
Progressively moved down when carrying out neutralization reaction, mixed with DOTP crude product and reaction time lengthening effect is more preferable.Plus
Thermal is simple and practical.Bottom heat pipe includes outer race tube, inner ring pipe and radial direction connecting leg, has the intensity of heating and enhancing kettle bottom surface concurrently
Effect.Side heat pipe and bottom heat pipe are semi-circular tube, and heating effect is good.Measuring pump is one kind of reciprocating pump, can adjust control
Flow processed.Neutralization reaction method makes liquid caustic soda mixed with DOTP crude product as the rotation of agitating paddle is progressively uniformly added into
Merge reaction, the time for reaching reaction end can be shortened and liquid caustic soda consumption is small.
The present invention can change into that various ways are apparent to one skilled in the art, and such change is not considered as
Depart from the scope of the present invention.All such technical staff to the field obviously change, and are included within this right
It is required that within the scope of.
Claims (1)
1. a kind of neutralization reaction method of neutralization reaction kettle, described neutralization reaction kettle, if including kettle, gusset stirred provided with dried layer
Mix oar and the main shaft being pivotally connected with kettle and the motor for being fixedly connected and being connected with spindle drive with kettle；It is characterized in that, it is described
Neutralization reaction kettle also includes liquid caustic soda pipe, pipeline swivel joint, liquid caustic soda delivery pump and heater；The gusset of main shaft is provided with several
Jet pipe；Main shaft is provided with the mesopore connected with lower surface insertion and with jet pipe；The lower end of main shaft passes through pipeline swivel joint and liquid caustic soda
One end connection of pipe；The other end of liquid caustic soda pipe stretches out the bottom of kettle and the outlet of liquid caustic soda delivery pump；Liquid caustic soda pipe and kettle
It is fixedly connected；The top of kettle is provided with charge door；The bottom of kettle is provided with drain hole；Heater include hotline heater,
It is wrapped on the outside of kettle gusset and the side heat pipe being fixedly connected with the gusset of kettle and the bottom heat being fixedly connected with the bottom surface of kettle
Pipe；The two ends of hotline heater are connected with one end of side heat pipe and one end of bottom heat pipe respectively；The other end of side heat pipe and bottom
The other end connection of heat pipe；Several described jet pipes are located at the most downside of last layer agitating paddle and radially equal along the gusset of main shaft
Cloth；The upside of each jet pipe gusset is provided with least one liquid caustic soda nozzle；Described bottom heat pipe includes outer race tube, inner ring pipe and some
The individual radial direction connecting leg for being uniformly distributed along the circumference and being connected respectively with outer race tube and inner ring pipe；Described side heat pipe is semi-circular tube；Bottom heat pipe
For semi-circular tube；Described liquid caustic soda delivery pump is measuring pump；It is characterized in that：（1）The DOTP crude product of specified quantity
Added from charge door in kettle；（2）Open motor and drive agitating paddle stirring DOTP crude product；（3）In agitating paddle
In the state of stirring and jet pipe are rotated, hotline heater is opened, conduction oil is by side heat pipe and bottom heat pipe to pair in kettle
Dioctyl phthalate crude product heat temperature raising；（4）Liquid caustic soda delivery pump is opened, liquid caustic soda is under liquid caustic soda conveying pumping action through mesopore from spray
Pipe sprays to enter to be mixed in kettle with DOTP crude product, until reaching the rule with DOTP crude product
Fixed proportioning；（5）When the mixed liquid temperature degree of DOTP crude product and liquid caustic soda reaches 110 DEG C, isothermal reaction is kept, until in
Reaction end, and stratification are reached with reaction；（6）By drain hole by DOTP, para-phthalic sodium and
Water stratification is released.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310187925.7A CN104174348B (en) | 2013-05-20 | 2013-05-20 | Neutralization reaction kettle and neutralization reaction method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310187925.7A CN104174348B (en) | 2013-05-20 | 2013-05-20 | Neutralization reaction kettle and neutralization reaction method |
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| Publication Number | Publication Date |
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| CN104174348A CN104174348A (en) | 2014-12-03 |
| CN104174348B true CN104174348B (en) | 2017-07-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310187925.7A Active CN104174348B (en) | 2013-05-20 | 2013-05-20 | Neutralization reaction kettle and neutralization reaction method |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109678712A (en) * | 2019-01-29 | 2019-04-26 | 安徽力天环保科技股份有限公司 | A kind of dioctyl phthalate preparation facilities and preparation method thereof |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1749050A2 (en) * | 1990-05-29 | 1992-07-23 | Рижский политехнический институт | Device for aeration of mixed materials |
| JPH09117654A (en) * | 1995-10-24 | 1997-05-06 | Ishikawajima Harima Heavy Ind Co Ltd | Washing device for agitating tank |
| US6491423B1 (en) * | 1998-03-11 | 2002-12-10 | Mc21, Incorporated | Apparatus for mixing particles into a liquid medium |
| DE102004010146B4 (en) * | 2004-02-27 | 2006-02-16 | Zimmer Ag | Process and apparatus for the production of polyesters and copolyesters |
| CN102039111A (en) * | 2009-10-10 | 2011-05-04 | 武建民 | Continuous hydrolysis kettle converted from furfural intermittent hydrolysis kettle |
| EP2826548B1 (en) * | 2010-03-03 | 2017-10-18 | Zacharias Joseph Van Den Berg | Waste water treatment system |
| CN203316122U (en) * | 2013-05-20 | 2013-12-04 | 宁波凯诚环保科技有限公司 | Neutralization reaction kettle |
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