CN207775117U - Continuous device is washed in the neutralization of citrate - Google Patents
Continuous device is washed in the neutralization of citrate Download PDFInfo
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- CN207775117U CN207775117U CN201721901679.7U CN201721901679U CN207775117U CN 207775117 U CN207775117 U CN 207775117U CN 201721901679 U CN201721901679 U CN 201721901679U CN 207775117 U CN207775117 U CN 207775117U
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Abstract
The utility model provides a kind of neutralization washing continuous device of citrate, continuous device is washed in the neutralization of specially a kind of tributyl 2-acetylcitrate, the neutralization washing continuous device includes thick ester tank, heater, extracting tower, condenser, acid storage tank, neutralize kettle, centrifuge, return water tank, washing kettle, drying tower, ester holding vessel, waste water desalination tower, the device passes through extracting tower, kettle is neutralized to remove the acetic acid in tributyl 2-acetylcitrate, acetic anhydride and catalyst sulfuric acid hydrogen sodium acid impurities, it washes again and removes the organic salt that acid impurities react generation with alkali, last drier removes moisture and obtains refined tributyl 2-acetylcitrate.
Description
Technical field
The utility model belongs to plasticizer manufacturing technology field, and in particular to a kind of neutralization water of tributyl 2-acetylcitrate
Wash continuous device.
Background technology
Two principal item tributyl citrate, tributyl 2-acetylcitrates of citrate, wherein acetyl tributyl citrate three
N-butyl, abbreviation ATBC, molecular formula C20H34O8, structural formula is as shown below, and sterling is colourless, tasteless oily liquid
Body, 343 DEG C of boiling point；Acetyl tri-n-butyl citrate (ATBC) be a kind of novel asepsis environment-protecting plasticizer, have it is non-toxic and tasteless,
Compatibility is good, plasticizing efficiency is high, is easily biodegradable the advantages that small with volatility, cold resistance, light resistance and has excellent water-resistance, can
Substitute phthalate conventional plasticizers.The plasticizer that can be used as polyvinyl chloride, celluosic resin and synthetic rubber, is used for
The products such as nontoxic PVC granulations, food container, toy for children product, medical product, film, plank, cellulose paint,
The stabilizer etc. that can be used as polyvinylidene chloride is a kind of important chemical products.
The preparation of usual tributyl 2-acetylcitrate is first by citric acid, n-butanol in concentrated sulfuric acid catalyst, temperature 110
The lower reaction of~150 DEG C of effects generates tributyl citrate crude product, contains the complete lemon of unreacted in tributyl citrate crude product at this time
Lemon acid and n-butanol impurity and the catalyst concentrated sulfuric acid, it is general use quality is added as concentrated sulfuric acid quality 60~85% alkali with
The catalyst neutralisation concentrated sulfuric acid and unreacted citric acid, then high temperature serialization dealcoholysis obtain the higher tributyl citrate of precision,
It is later that the higher tributyl citrate of precision and acetic anhydride is anti-in the case where catalyst sulfuric acid hydrogen sodium, temperature are 50~100 DEG C of effects
Tributyl 2-acetylcitrate crude product should be generated, tributyl citrate can be made to convert substantially completely, avoid tributyl citrate
Detach difficult problem with tributyl 2-acetylcitrate, but the tributyl 2-acetylcitrate crude product contains acetic anhydride, generates
Acetic acid, niter cake acid impurities, the tributyl 2-acetylcitrate for containing impurity are added to as plasticizer in plastics, can be serious
The performance of plastics is influenced, therefore needs a kind of device that can neutralize the impurity in washing tributyl 2-acetylcitrate at present.
Utility model content
For the above situation, to overcome the defect of the prior art, the utility model to provide a kind of neutralization water of citrate
Wash continuous device, continuous device is washed in the neutralization of specially a kind of tributyl 2-acetylcitrate, the device by extracting tower,
Kettle is neutralized to remove the acetic acid in tributyl 2-acetylcitrate, acetic anhydride and catalyst sulfuric acid hydrogen sodium acid impurities, then washes and removes
Acid impurities are gone to react the organic salt generated with alkali, last drier removes moisture and obtains refined tributyl 2-acetylcitrate.
The utility model provides a kind of neutralization washing continuous device of citrate, and continuous device is washed in the neutralization
Including thick ester tank, heater, extracting tower, condenser, acid storage tank, neutralize kettle, centrifuge, return water tank, washing kettle, drying tower,
Ester holding vessel, waste water desalination tower, wherein
(1) the first overflow pipe from below to up drawn from the thick ester pot bottom accesses the heater lower part, described
First pipeline derived from the top of heater accesses the extracting tower lower part, and the second pipeline access derived from the extracting tower top is suitable
Secondary concatenated first condenser, acid storage tank, the second overflow pipe that the depickling tower bottom is drawn access the neutralization kettle；
(2) pipeline for neutralizing kettle top portion and being equipped with access lye delivery device, draws from the lower part for neutralizing kettle
Third overflow pipe accesses the first centrifuge, and the third pipeline that the lower part of first centrifuge is drawn accesses the washing kettle, institute
State the 4th pipeline access return water tank that the top of the first centrifuge is drawn；
(3) it is equipped with the pipeline for accessing the solvent device that aborts at the top of the washing kettle, is drawn from the lower part of the washing kettle
The 4th overflow pipe access the second centrifuge, the top for the 5th pipeline access drying tower that the lower part of second centrifuge is drawn
Portion, the 6th pipeline that the top of second centrifuge is drawn access return water tank；
(4) the 5th overflow pipe that the dry tower bottom is drawn accesses ester holding vessel；
(5) water pipe that the return water tank lower part picks out is pumped into waste water desalination tower in booster pump.
Preferably, the second overflow pipe that the depickling tower bottom is drawn accesses at least two neutralization kettles in sequential series, institute
It states and neutralizes third overflow pipe the first centrifuge of access that the lower part of kettle is drawn, the third pipe of the lower part extraction of first centrifuge
Next neutralization kettle is accessed on road, and the 4th pipeline that the top of first centrifuge is drawn accesses return water tank.
Preferably, the third pipeline that the lower part of first centrifuge is drawn accesses at least two washings in sequential series
Kettle, the 4th overflow pipe that the lower part of the washing kettle is drawn access the second centrifuge, second centrifuge lower part draw the
Five pipelines access next washing kettle, and the 6th pipeline that the top of second centrifuge is drawn accesses return water tank.
Preferably, it is equipped with agitating device in the neutralization kettle and the washing kettle.
Preferably, the depickling tower bottom is equipped with reboiler, the second overflow pipe access drawn from the reboiler bottom
The neutralization kettle.
Preferably, the water pipe that the return water tank lower part picks out is pumped into waste water desalination tower in booster pump, and the waste water is de-
The 7th pipeline that salt tower bottom is drawn accesses organic salt holding vessel, the 8th pipeline access that the waste water desalination top of tower is drawn the
Two condensers, reclaim liquid phase waste water.
Preferably, 5A molecular sieves and calcium chloride drier alternating layer paving is laid with from bottom to up in the drying tower.
The utility model provides a kind of neutralization washing continuous device of citrate, specially a kind of acetyl tributyl citrate three
Continuous device is washed in the neutralization of butyl ester, and the device is by extracting tower, neutralization kettle and to remove in tributyl 2-acetylcitrate
Acetic acid, acetic anhydride and niter cake acid impurities, then reacted by washing kettle with to remove acid impurities with alkali the organic salt generated,
Last drying tower dries and removes moisture and obtains refined tributyl 2-acetylcitrate.The apparatus structure is simple, easy to operate, product production
Amount is big, and stable quality, the degree of automation is higher, saves a large amount of human costs, increases the processing that condenser removes acid tail gas
Device has prevented pollution of the acid waste gas to air, and has been equipped with waste water desalination tower, it is therefore prevented that water pollution solves environment guarantor
Shield problem.
Description of the drawings
Fig. 1 is the structure chart of the neutralization washing continuous device of citrate in the utility model.
Specific implementation mode
Specific embodiment of the present utility model is described in further detail below in conjunction with attached drawing, to enable art technology
Personnel can implement according to this with reference to specification word.
It should be appreciated that such as " having ", " comprising " term used herein does not allot one or more of the other element
Or combinations thereof presence or addition.It should be noted that device described in following proposal and material, unless otherwise specified,
It obtains from commercial channels.
As shown in Figure 1, the utility model provides a kind of neutralization washing continuous device of citrate, the neutralization washing
Continuous device includes thick ester tank 1, heater 2, extracting tower 4, the first condenser 6, acid storage tank 7, neutralizes kettle 8, centrifuge 10, returns
Receive water tank 16, washing kettle 11, drying tower 14, ester holding vessel 15, waste water desalination tower 18, wherein
(1) the first overflow pipe from below to up drawn from thick 1 bottom of ester tank accesses 2 lower part of heater, institute
It states the first pipeline derived from the top of heater 2 and accesses 4 lower part of extracting tower, the second pipeline derived from 4 top of the extracting tower
The first condenser 6 in sequential series, acid storage tank 7 are accessed, the second overflow pipe access that 4 bottom of the extracting tower is drawn neutralizes kettle 8；
(2) pipeline for neutralizing 8 top of kettle and being equipped with access lye delivery device 9, draws from the lower part for neutralizing kettle 8
The third overflow pipe gone out accesses the first centrifuge 10, and the third pipeline that the lower part of first centrifuge 10 is drawn accesses the water
Kettle 11 is washed, the 4th pipeline that the top of first centrifuge 10 is drawn accesses return water tank 16；
(3) 11 top of the washing kettle is equipped with the pipeline for accessing the solvent device 12 that aborts, under the washing kettle 11
The 4th overflow pipe that portion is drawn accesses the second centrifuge 13, and the 5th pipeline access that the lower part of second centrifuge 13 is drawn is dry
The top of dry tower 14, the 6th pipeline that the top of second centrifuge 13 is drawn access return water tank 16；
(4) the 5th overflow pipe access ester holding vessel 15 that 14 bottom of the drying tower is drawn；
(5) water pipe that 16 lower part of the return water tank picks out is pumped into waste water desalination tower 18, the waste water in booster pump 17
The 7th pipeline access organic salt holding vessel 20 that 18 bottom of desalination tower is drawn, the 8th pipe of 18 Base top contact of waste water desalination tower
The second condenser 19, reclaim liquid phase waste water are accessed in road.
In the technical solution of the utility model, the second overflow pipe that 4 bottom of the extracting tower is drawn accesses at least two
Neutralization kettle 8 in sequential series, third overflow pipe the first centrifuge 10 of access that the lower part for neutralizing kettle 8 is drawn, described first
The third pipeline that the lower part of centrifuge 10 is drawn accesses next neutralization kettle 8 ', and the top of first centrifuge 10 is drawn
The 4th pipeline access return water tank 16.The third pipeline access at least two that the lower part of first centrifuge 10 is drawn is sequentially
Concatenated washing kettle 11, the 4th overflow pipe that the lower part of the washing kettle 11 is drawn access the second centrifuge 13, described second from
The 5th pipeline that 13 lower part of scheming is drawn accesses next washing kettle 11 ', the top extraction of second centrifuge 13
6th pipeline accesses return water tank 16.It is equipped with agitating device in the neutralization kettle 8 and the washing kettle 11.The drying tower 14
Interior 5A molecular sieves are laid with from bottom to up with calcium chloride drier alternating layer paving.
The density 1.046g/cm of tributyl 2-acetylcitrate3(25 DEG C), 343 DEG C of boiling point (1 standard atmospheric pressure), do not dissolve in
Water is dissolved in most organic solvents.Acetic acid is a kind of colourless liquid having intense irritation tart flavour at normal temperatures, and density is
1.050g/cm3Boiling point 117.9 DEG C (391.2K), acetic acid is soluble easily in water and ethyl alcohol, aqueous solution are weakly acidic.Acetic anhydride is nothing
Color transparency liquid, density 1.080g/cm3There is strong acetic acid odor, it is sour, there is hygroscopicity, is dissolved in chloroform and ether, slowly
Ground is dissolved in water and forms acetic acid, 139 DEG C of boiling point.
Heating temperature in the heater 2 is 100~150 DEG C, and the vacuum degree of the extracting tower 4 is less than or equal to
10kPa, the temperature control at the top of the extracting tower 4 is at 100~140 DEG C, 5 heating temperature of reboiler of 4 bottom of the extracting tower
It is 140~160 DEG C, is 5~10% to neutralizing in kettle 8 through the concentration of lye that lye delivery device 9 is added, in described and water
Wash usual three neutralization kettles 8 in sequential series in continuous device, neutralize the concentration of lye being added in kettle 8 be successively followed successively by 9~
10%, 7~8%, 5~6%, then in each and kettle 8 in stir 30~40min, thick ester liquid from it is described neutralize kettle 8 lower part
The third overflow pipe of extraction flows into the first centrifuge 10, and the rotating speed of first centrifuge 10 is 600~800r/min, described
Usual two washing kettles 11 in sequential series in washing continuous device are neutralized, 10~20min is stirred in each washing kettle 11, is removed
The 4th overflow pipe that the tributyl 2-acetylcitrate liquid phase of acid impurities is drawn from the lower part of the washing kettle 11 is gone to flow into second
The rotating speed of centrifuge 13, second centrifuge 13 is 600~800r/min.
The aqueous alkali being added in kettle 11 that neutralizes is sodium carbonate, sodium hydroxide or sodium bicarbonate aqueous solution.
The thick ester liquid phase stored in the thick ester tank 1 enters heater 2 and is heated, and vapour is from the heater 2
Top output enters extracting tower 4, most acetic acid and acetic anhydride have been vaporized into gas phase in thick ester liquid phase, unboiled to steam
A small amount of acetic acid or acetic anhydride reheating in the reboiler 5 of 4 bottom of the extracting tower, by acetic acid or acetic anhydride heating vaporize into
Enter gas phase, gas phase, which enters after being condensed into liquid into the first condenser 6 in acid storage tank 7, to be stored.
Tributyl 2-acetylcitrate liquid phase flows into storage ester tank 15 after centrifuge, and water phase flows into return water tank 16, warp
Waste water is pumped into waste water desalination tower 18, and concentration ratio control is 4 in waste water desalination tower 18:1, the organic salt in waste water is concentrated,
It is discharged from waste water desalination tower 18, the waste water that tower top steams discharges after entering the further ester aqueous phase separation of cesspool.
Into the liquid shows neutral before drying tower, drier calcium chloride and 5A molecular sieves in drying tower absorb in liquid phase
Moisture, and 5A molecular sieves fully ensure that the porosity in the drying tower 14, obtain refined tributyl 2-acetylcitrate product.
It is not only in the description and the implementation although the embodiments of the present invention have been disclosed as above
Listed utilization, it can be applied to various fields suitable for the present invention completely, for those skilled in the art,
Other modifications may be easily implemented, therefore without departing from the general concept defined in the claims and the equivalent scope, this reality
It is not limited to specific details and legend shown and described herein with novel.
Claims (7)
1. continuous device is washed in a kind of neutralization of citrate, which is characterized in that the neutralization washes continuous device and includes
Thick ester tank, extracting tower, condenser, acid storage tank, neutralizes kettle, centrifuge, return water tank, washing kettle, drying tower, ester storage at heater
Tank, waste water desalination tower are deposited,
（One）The first overflow pipe from below to up drawn from the thick ester pot bottom accesses the heater lower part, the heating
First pipeline derived from the top of device accesses the extracting tower lower part, and the second pipeline access derived from the extracting tower top is sequentially gone here and there
The first condenser, the acid storage tank of connection, the second overflow pipe that the depickling tower bottom is drawn access the neutralization kettle；
（Two）The pipeline for neutralizing kettle top portion and being equipped with access lye delivery device, the third drawn from the lower part for neutralizing kettle
Overflow pipe accesses the first centrifuge, and the third pipeline that the lower part of first centrifuge is drawn accesses the washing kettle, and described the
The 4th pipeline that the top of one centrifuge is drawn accesses return water tank；
（Three）It is equipped with access at the top of the washing kettle to abort the pipeline of solvent device, the drawn from the lower part of the washing kettle
Four overflow pipes access the second centrifuge, the top of the 5th pipeline access drying tower of the lower part extraction of second centrifuge, institute
State the 6th pipeline access return water tank that the top of the second centrifuge is drawn；
（Four）The 5th overflow pipe that the dry tower bottom is drawn accesses ester holding vessel；
（Five）The water pipe that the return water tank lower part picks out is pumped into waste water desalination tower in booster pump.
2. continuous device is washed in the neutralization of citrate according to claim 1, which is characterized in that the extracting tower bottom
The second overflow pipe that portion is drawn accesses at least two neutralization kettles in sequential series, the third overflow that the lower part for neutralizing kettle is drawn
Pipe accesses the first centrifuge, and the third pipeline that the lower part of first centrifuge is drawn accesses next neutralization kettle, described
The 4th pipeline that the top of first centrifuge is drawn accesses return water tank.
3. continuous device is washed in the neutralization of citrate according to claim 1, which is characterized in that first centrifugation
Third pipeline at least two washing kettles in sequential series of access that the lower part of machine is drawn, the 4th of the lower part extraction of the washing kettle the
Overflow pipe accesses the second centrifuge, and the 5th pipeline that second centrifuge lower part is drawn accesses next washing kettle, institute
State the 6th pipeline access return water tank that the top of the second centrifuge is drawn.
4. continuous device is washed in the neutralization of citrate according to claim 1, which is characterized in that the neutralizations kettle with
It is equipped with agitating device in the washing kettle.
5. continuous device is washed in the neutralization of citrate according to claim 1, which is characterized in that the extracting tower bottom
Portion is equipped with reboiler, and the second overflow pipe drawn from the reboiler bottom accesses the neutralization kettle.
6. continuous device is washed in the neutralization of citrate according to claim 1, which is characterized in that the return water tank
The water pipe that lower part picks out is pumped into waste water desalination tower in booster pump, and the 7th pipeline access that the waste water desalination tower bottom is drawn has
Machine salt holding vessel, the 8th pipeline that the waste water desalination top of tower is drawn access the second condenser, reclaim liquid phase waste water.
7. continuous device is washed in the neutralization of citrate according to claim 1, which is characterized in that in the drying tower
5A molecular sieves are laid with from bottom to up with calcium chloride drier alternating layer paving.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721901679.7U CN207775117U (en) | 2017-12-29 | 2017-12-29 | Continuous device is washed in the neutralization of citrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721901679.7U CN207775117U (en) | 2017-12-29 | 2017-12-29 | Continuous device is washed in the neutralization of citrate |
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| Publication Number | Publication Date |
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| CN207775117U true CN207775117U (en) | 2018-08-28 |
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| CN201721901679.7U Expired - Fee Related CN207775117U (en) | 2017-12-29 | 2017-12-29 | Continuous device is washed in the neutralization of citrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807920A (en) * | 2020-07-14 | 2020-10-23 | 中国石油化工股份有限公司 | Method and system for deacidifying cumene raw material of CHPPO (chlorinated Polypropylene oxide) device |
-
2017
- 2017-12-29 CN CN201721901679.7U patent/CN207775117U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807920A (en) * | 2020-07-14 | 2020-10-23 | 中国石油化工股份有限公司 | Method and system for deacidifying cumene raw material of CHPPO (chlorinated Polypropylene oxide) device |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180828 Termination date: 20191229 |