CN107778170A - A kind of isobutyl palmitate production system - Google Patents

A kind of isobutyl palmitate production system Download PDF

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Publication number
CN107778170A
CN107778170A CN201610733233.1A CN201610733233A CN107778170A CN 107778170 A CN107778170 A CN 107778170A CN 201610733233 A CN201610733233 A CN 201610733233A CN 107778170 A CN107778170 A CN 107778170A
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CN
China
Prior art keywords
tank
retort
steam
storage tank
isobutyl palmitate
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Pending
Application number
CN201610733233.1A
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Chinese (zh)
Inventor
刘海波
江海
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Zhijiang Yi Yi Chemical Co Ltd
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Zhijiang Yi Yi Chemical Co Ltd
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Priority to CN201610733233.1A priority Critical patent/CN107778170A/en
Publication of CN107778170A publication Critical patent/CN107778170A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

Abstract

A kind of isobutyl palmitate production system; including esterification part and purification part, by palmitic acid and isooctanol in retort frequent esterification, reaction when be filled with nitrogen protection; most isooctanol can be proposed by the first condenser and oil water separator, and isobutyl palmitate crude product is made；Isobutyl palmitate crude product is pumped into purification tank again it is evaporated under reduced pressure, propose wherein unnecessary moisture, hexamethylene and isooctanol, isobutyl palmitate finished product is made；Due to being heated using nitrogen protection and steam, therefore reaction condition is constant, and the reaction time is controllable, obtains isobutyl palmitate good product quality, clear；Unnecessary isooctanol, hexamethylene and the catalyst proposed during reaction can recycle, and reduce entreprise cost；The waste gas of discharge is filtered by bubbling tank, reduces environmental pollution.

Description

A kind of isobutyl palmitate production system
Technical field
Of the invention and a kind of isobutyl palmitate production system.
Background technology
Isobutyl palmitate is the product that palmitic acid and isooctanol acetify reaction, needs to add catalyst in production And hexamethylene, 2% to 50% water, unreacted catalyst, cyclohexane and different can be contained in the isobutyl palmitate produced Octanol, it is therefore desirable to which purification is carried out to isobutyl palmitate crude product to be used, usually using ternary public affairs boiling method and the way of distillation Purified, not only equipment investment is big for this method of purification, complex operation, and the isobutyl palmitate purity purified out is not It is high.
The content of the invention
The technical problem to be solved in the present invention provides a kind of isobutyl palmitate production system, can generate high-purity Isobutyl palmitate, equipment investment is small, easy to operate, and caused waste can recycle in process of production.
In order to solve the above-mentioned technical problem, the technical scheme is that：A kind of isobutyl palmitate production system, including Esterification part and purification part,
Esterification part：Including retort, palm acid storage tank, isooctanol storage tank, hexamethylene storage tank, nitrogen cylinder, the first condensation Device, oil water separator, catalyst storage tank, agitating device and the first steam generator；Palm acid storage tank, isooctanol storage tank and hexamethylene Alkane storage tank is provided with measuring pump, flowmeter and valve respectively by a feed tube connection at the top of retort on feed tube, Nitrogen cylinder is connected at the top of retort by pipeline communication in reaction pot bottom, the import of the first condenser by blast pipe, the The outlet of one condenser connects the import in oil water separator by escape pipe, and the oil-out of oil water separator is connected by oil return pipe Lead to and connected in the top of isooctanol storage tank, the delivery port of oil water separator with a drainpipe, catalyst storage tank passes through duff pipe Connection is at the top of retort；
Agitating device includes being arranged on the motor above retort, and a stirring is fixed with the rotating shaft of motor Axle, one end of agitating shaft are extended in retort through reaction tank wall, and being located at one end in retort in agitating shaft is fixed with Multiple agitating paddles；
The retort is inside and outside two layers, is left between internal layer and outer layer for steam-heated first gap, the first steam generation The steam (vapor) outlet of device is connected by the first steam pipe with the first gap, and the first gap is connected by the first steam discharge pipe with extraneous It is logical；
Purify part：Steamed including centrifugal pump, filter, purification tank, the second condenser, hydrops tank, bubbling tank, vacuator and second Vapour generator, purification pot bottom are arranged on liquid suction pipe by taking out liquid line connection in reaction pot bottom, filter and centrifugal pump, The inlet communication of second condenser is crossed tracheae by one respectively and connected in purification tank top, the outlet of the second condenser and bubbling tank Lead in hydrops tank top, return pump is by an exhaust tube connection at the top of bubbling tank；
The purification tank is inside and outside two layers, is left between internal layer and outer layer for steam-heated second gap, the second steam generation The steam (vapor) outlet of device is connected by the second steam pipe with the second gap, and the second gap is connected by the second steam discharge pipe with extraneous It is logical.
Feed tube one end is extended to inside retort through reaction tank wall, one end peace being located in feed tube in retort Equipped with water-locator.
Vibrator is installed on catalyst storage tank.
Aeration tube is laid with bubbling tank tank bottom, tracheae one end is crossed and is connected through bubbling tank wall with aeration tube.
A sampling pipe is communicated with the middle part of retort.
The beneficial effects of the invention are as follows：By palmitic acid and isooctanol in retort frequent esterification, reaction when fill Enter nitrogen protection, most isooctanol can be proposed by the first condenser and oil water separator, and isobutyl palmitate crude product is made； Isobutyl palmitate crude product is pumped into purification tank again it is evaporated under reduced pressure, propose wherein unnecessary moisture, hexamethylene And isooctanol, the isobutyl palmitate finished product of obtained high-purity；Due to being heated using nitrogen protection and steam, therefore reaction condition Constant, the reaction time is controllable, obtains isobutyl palmitate good product quality, clear；What is proposed during reaction is unnecessary different pungent Alcohol, hexamethylene and catalyst can recycle, and reduce entreprise cost；The waste gas of discharge is filtered by bubbling tank, dropped Low environmental pollution.
Brief description of the drawings
The present invention is described further below in conjunction with the accompanying drawings：
Fig. 1 is the structural representation of the present invention,
Fig. 2 is close-up schematic view of the present invention on retort,
Fig. 3 is close-up schematic view of the present invention on bubbling tank.
In figure:Isooctanol storage tank 1, palm acid storage tank 2, hexamethylene storage tank 3, nitrogen cylinder 4, sampling pipe 5, retort 6, One steam generator 7, centrifugal pump 8, filter 9, the second steam generator 10, purification tank 11, the second steam discharge pipe 12, bubbling Tank 13, vacuator 14, aeration tube 15, hydrops tank 16, the second condenser 17, oil water separator 18, the first condenser 19, catalyst Storage tank 20, motor 21, water-locator 22, the first steam discharge pipe 23, flowmeter 24, measuring pump 25, the first gap 61, second Gap 111, clear water enter pipe 131, fluid delivery pipe 132, clear water delivery pipe 133, agitating shaft 211, agitating paddle 212.
Embodiment
A kind of isobutyl palmitate production system, including esterification part and purification part,
Esterification part：Including retort 6, palm acid storage tank 2, isooctanol storage tank 1, hexamethylene storage tank 3, nitrogen cylinder 4, first Condenser 19, oil water separator 18, catalyst storage tank 20, agitating device and the first steam generator 7；It is palm acid storage tank 2, different pungent Alcohol storage tank 1 is connected at the top of retort 6 by a feed tube respectively with hexamethylene storage tank 3, and metering is provided with feed tube Pump 25, flowmeter 24 and valve, nitrogen cylinder 4 pass through row by pipeline communication in the bottom of retort 6, the import of the first condenser 19 Tracheae connection is exported by escape pipe connection in the import of oil water separator 18, oil in the top of retort 6, the first condenser 19 The oil-out of separator 18 is connected in the top of isooctanol storage tank 1, the delivery port of oil water separator 18 and one by oil return pipe Root drainpipe is connected, and catalyst storage tank 20 is connected at the top of retort 6 by duff pipe；
Agitating device includes the motor 21 for being arranged on the top of retort 6, and one is fixed with the rotating shaft of motor 21 Agitating shaft 211, one end of agitating shaft 211 are extended in retort 6 through the outer wall of retort 6, are located at retort in agitating shaft 211 One end in 6 is fixed with multiple agitating paddles 212；
The retort 6 is inside and outside two layers, is left between internal layer and outer layer for steam-heated first gap 61, the first steam hair The steam (vapor) outlet of raw device 7 is connected by the first steam pipe with the first gap 61, and the first gap 61 passes through the first steam discharge pipe 23 It is in communication with the outside, the heat-preservation cotton for being incubated is coated with retort.
Purify part：Including centrifugal pump 8, filter 9, purification tank 11, the second condenser 17, hydrops tank 16, bubbling tank 13, The steam generator 10 of vacuator 14 and second, the purification bottom of tank 11 is by taking out liquid line connection in the bottom of retort 6, filter 9 It is arranged on centrifugal pump 8 on liquid suction pipe, the inlet communication of the second condenser 17 goes out in the top of purification tank 11, the second condenser 17 Mouth is crossed tracheae by one respectively with bubbling tank 13 and connected at the top of hydrops tank 16, and return pump is by an exhaust tube connection in drum Steep the top of tank 13；
The purification tank 11 is inside and outside two layers, is left between internal layer and outer layer for steam-heated second gap 111, the second steam The steam (vapor) outlet of generator 10 is connected by the second steam pipe with the second gap 111, and the second gap 111 passes through the second discharge of steam Pipe 12 is in communication with the outside, and drainage conduit is communicated with purification tank 11 bottom.
Clear water is communicated with the top of bubbling tank 13 and enters pipe 131, middle part is communicated with fluid delivery pipe 132, and bottom is communicated with Clear water delivery pipe 133.
The workflow and principle of the present invention：Add in palm acid solution, isooctanol storage tank 1 and add in palm acid storage tank 2 Enter to add in isooctanol solution, hexamethylene storage tank 3 and stannous oxalate solid acid catalysis is added in cyclohexane solution, catalyst storage tank 20 Agent.
Open the first steam generator 7 160 degree of high-temperature steams are passed into the first gap 61, keep the temperature of retort 6 More than 150 degree, each measuring pump 25 and valve are opened by palm acid solution, isooctanol solution, cyclohexane solution and catalyst It is circulated into according to a certain percentage in retort 6 and carries out esterification, while opens motor 21 and the solution in retort 6 is entered Row stirring, nitrogen is then passed into by progress nitrogen protection in retort 6 by nitrogen cylinder 4, generates isobutyl palmitate crude product, The first condenser 19, the first condenser 19 are entered by blast pipe after isooctanol, vapor and nitrogen mixing during the course of the reaction Condense gas into oily liq and be drained into oil water separator 18 and carry out water-oil separating, oil water separator 18 is isolated different pungent Alcohol is back in isooctanol storage tank 1 by oil return pipe and reused, and the water that oil water separator 18 is isolated is discharged from drainpipe.
After esterification partial reaction 5 hours, the first steam generator 7, measuring pump 25, motor 21 and valve are closed Door, 150 degree are heated to by tank 11 is purified by the second steam generator 10, is then turned on centrifugal pump 8 by the palm in retort 6 In the different monooctyl ester crude product purification tank 11 of acid, when purifying isobutyl palmitate solution of the tank 11 equipped with 2/3rds volumes, centrifugal pump 8 It is stopped, while when isobutyl palmitate crude product passes through filter 9, filter 9 can filter out stannous oxalate solid acid Catalyst；Then vacuator 14 will purify tank 11 and be evacuated to negative pressure, and isobutyl palmitate crude product can be because pressure reduces and temperature Raise and seethe with excitement, caused vapor can be entered in the second condenser 17 with the isooctanol and hexamethylene of residual and is cooled to The aqueous solution, the aqueous solution containing isooctanol and hexamethylene can be flowed into hydrops tank 16 and collect, and unnecessary vapor can pass through Bubbling tank 13 is washed, and when bubbling tank 13 is washed, the intermittence of vacuator 14 is opened and closed, and the gas in bubbling tank 13 is extracted out.
Isobutyl palmitate after being purified can discharge from drainage conduit 12.
After precipitation, isooctanol can be swum on the water surface solution in bubbling tank 13, can pass through fluid delivery pipe 132 Isooctanol discharge is being utilized.
Because the present invention is heated using steam, therefore heating-up temperature constant homogeneous, isobutyl palmitate esterification is improved Reaction and refining effect, and the stannous oxalate solid acid in caused excess isooctanol and filter 9 is urged in process of production Agent can sufficiently be reclaimed and utilized, and save production cost, the vapor of discharge can be entered by bubbling tank 13 in addition Row filtering, reduces environmental pollution.
Feed tube one end is extended to inside retort 6 through the outer wall of retort 6, is located at one in retort 6 in feed tube End is provided with water-locator 22, and water-locator 22 can enable solution to be dispersed into retort 6.
Vibrator is installed on catalyst storage tank 20, vibrator being discharged into favor of grained catalyst.
Aeration tube 15 is laid with the tank bottom of bubbling tank 13, tracheae one end is crossed and connects through the outer wall of bubbling tank 13 with aeration tube 15 Logical, aeration tube 15 can improve water washing effect.
A sampling pipe 5 is communicated with the middle part of retort 6, can be very easily by retort 6 by sampling pipe 5 Solution discharge out often detection.
In summary：The present invention is using nitrogen protection and steam heating, therefore reaction condition is constant, and the reaction time is controllable, Obtain isobutyl palmitate good product quality, clear；Unnecessary isooctanol, hexamethylene and the catalyst proposed during reaction can To recycle, entreprise cost is reduced；The waste gas of discharge is filtered by bubbling tank 13, reduces environmental pollution.

Claims (5)

  1. A kind of 1. isobutyl palmitate production system, it is characterised in that：Including esterification part and part is purified,
    Esterification part：Including retort（6）, palm acid storage tank（2）, isooctanol storage tank（1）, hexamethylene storage tank（3）, nitrogen Bottle（4）, the first condenser（19）, oil water separator（18）, catalyst storage tank（20）, agitating device and the first steam generator （7）；Palm acid storage tank（2）, isooctanol storage tank（1）With hexamethylene storage tank（3）Respectively by a feed tube connection in retort （6）Top, measuring pump is installed on feed tube（25）, flowmeter（24）And valve, nitrogen cylinder（4）By pipeline communication anti- Answer tank（6）Bottom, the first condenser（19）Import by blast pipe connect in retort（6）Top, the first condenser（19） Outlet by escape pipe connect in oil water separator（18）Import, oil water separator（18）Oil-out connected by oil return pipe Lead in isooctanol storage tank（1）Top, oil water separator（18）Delivery port connected with a drainpipe, catalyst storage tank（20） Connected by duff pipe in retort（6）Top；
    Agitating device includes being arranged on retort（6）The motor of top（21）, in motor（21）Rotating shaft on it is fixed There is an agitating shaft（211）, agitating shaft（211）One end pass through retort（6）Outer wall extends to retort（6）It is interior, stirring Axle（211）Positioned at retort（6）Interior one end is fixed with multiple agitating paddles（212）；
    The retort（6）For inside and outside two layers, left between internal layer and outer layer for steam-heated first gap（61）, first steams Vapour generator（7）Steam (vapor) outlet pass through the first steam pipe and the first gap（61）Connection, the first gap（61）Steamed by first Vapour delivery pipe（23）It is in communication with the outside；
    Purify part：Including centrifugal pump（8）, filter（9）, purification tank（11）, the second condenser（17）, hydrops tank（16）, drum Steep tank（13）, vacuator（14）With the second steam generator（10）, purify tank（11）Reacted by taking out liquid line connection bottom Tank（6）Bottom, filter（9）And centrifugal pump（8）On liquid suction pipe, the second condenser（17）Inlet communication purification tank （11）Top, the second condenser（17）Outlet and bubbling tank（13）Tracheae connection is crossed in hydrops tank by one respectively（16）Top Portion, return pump is by an exhaust tube connection in bubbling tank（13）Top；
    The purification tank（11）For inside and outside two layers, left between internal layer and outer layer for steam-heated second gap（111）, second Steam generator（10）Steam (vapor) outlet pass through the second steam pipe and the second gap（111）Connection, the second gap（111）Pass through Two steam discharge pipes（12）It is in communication with the outside.
  2. A kind of 2. isobutyl palmitate production system according to claim 1, it is characterised in that：Feed tube one end is through instead Answer tank（6）Outer wall extends to retort（6）Inside, it is located at retort in feed tube（6）Interior one end is provided with water-locator（22）.
  3. A kind of 3. isobutyl palmitate production system according to claim 1, it is characterised in that：In catalyst storage tank（20） On vibrator is installed（201）.
  4. A kind of 4. isobutyl palmitate production system according to claim 1, it is characterised in that：In bubbling tank（13）Tank bottom It is laid with aeration tube（15）, cross tracheae one end and pass through bubbling tank（13）Outer wall and aeration tube（15）Connection.
  5. A kind of 5. isobutyl palmitate production system according to claim 1, it is characterised in that：In retort（6）In Portion is communicated with a sampling pipe（5）.
CN201610733233.1A 2016-08-27 2016-08-27 A kind of isobutyl palmitate production system Pending CN107778170A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610733233.1A CN107778170A (en) 2016-08-27 2016-08-27 A kind of isobutyl palmitate production system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610733233.1A CN107778170A (en) 2016-08-27 2016-08-27 A kind of isobutyl palmitate production system

Publications (1)

Publication Number Publication Date
CN107778170A true CN107778170A (en) 2018-03-09

Family

ID=61438465

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610733233.1A Pending CN107778170A (en) 2016-08-27 2016-08-27 A kind of isobutyl palmitate production system

Country Status (1)

Country Link
CN (1) CN107778170A (en)

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Application publication date: 20180309

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