CN105037147B - A kind of production method of n-propyl acetate - Google Patents
A kind of production method of n-propyl acetate Download PDFInfo
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- CN105037147B CN105037147B CN201510436365.3A CN201510436365A CN105037147B CN 105037147 B CN105037147 B CN 105037147B CN 201510436365 A CN201510436365 A CN 201510436365A CN 105037147 B CN105037147 B CN 105037147B
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- propyl acetate
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- scalp pomade
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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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of production method of n-propyl acetate is it is characterised in that described step is：Acetic acid and propanol preheated rear entrance react generation n-propyl acetate in esterification column, obtain thick n-propyl acetate through condensing；Send into treating column after thick n-propyl acetate preheating and n-propyl acetate finished product is obtained in bottom of towe；Treating column top gaseous phase thing is sent in scalp pomade tank after partial condensation, includes liquid and gas in scalp pomade tank simultaneously：Scalp pomade tank internal upper part is low boiling gaseous component, controls scalp pomade pressure tank, and then by pipeline, low boiling gaseous component is passed directly into the continuation participation reaction of esterification column bottom.Provide part of heat energy for reaction, the yield of product can be effectively improved, reduce the energy being lost because low boiling point component circulates in refining system for a long time；Meanwhile, by controlling the pressure of scalp pomade tank, the heating for esterification that treating column gas phase is stable can be made, increased the stable of system and operability.
Description
Technical field
The present invention relates to a kind of manufacture method of ester, particularly to a kind of production method of n-propyl acetate.
Background technology
N-propyl acetate is the acetass of the common lower aliphatic alcohols of a class, frequently as coating, ink, nitro spray painting, clear
Paint and the fine solvent of various resin, are also applied to essence and flavoring agent industry.
With the requirement more and more higher of energy-conservation and environmental protection, the manufacturing enterprise of n-propyl acetate also increasingly pays close attention to acetic acid positive third
The energy consumption of ester production process declines.And the price competition of these conventional products is more and more fierce, this requires that manufacturing enterprise needs
Continuously search for reducing the road of production cost, thus the technique that more efficient energy-saving continually developed by manufacturing enterprise's needs.
In n-propyl acetate product processes traditional at present, raw material propyl ester and acetic acid through peracetic acid feed exchanger and
Esterification reboiler is entered, esterification reboiler makes material gasification extremely be esterified through steam heating after the preheating of propanol feed exchanger
Tower, generates thick n-propyl acetate, the thick n-propyl acetate of esterification column overhead extraction through reaction under catalyst action in esterification column
Enter rectifying column after reboiler heating, the gas phase containing light component, from refined overhead extraction, enters after condenser cooling
Scalp pomade tank, refined tower bottom produces finished product n-propyl acetate.
According to the production technology of above-mentioned traditional n-propyl acetate, there is no the process what heat makes full use of, esterification needs
Consume considerable steam, the energy consumption of esterification moiety will account for the 40～50% of whole production energy consumption, refined tower top
Vapor condensation is also required to substantial amounts of recirculated water；Thick ester enters rectifying column without prior preheating, easily causes caloic in tower to pass
The disorder passed, the oil phase of pump to overhead reflux, without prior preheating, also can be quenched the partial gas phase of tower top, increases bottom of towe again
The load of boiling device, causes the reduction of rectifying column separation efficiency；Formed after the low-boiling point alcohol brought into by raw alcohol and acid esterification
Some lower boiling impurity esters circulate always with oil phase in refining system, and only small part reenters reaction system from scalp pomade
System, a large portion comes back to treating column, increases the energy consumption of refining system.
Deficiency for existing n-propyl acetate production system can reduce energy in production process it is necessary to develop one kind
The method of consumption.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of production method of n-propyl acetate, not only can discharge in time
Fall some low boiling impurities in system, and reduced by the energy consumption that the coupling of heat exchange amount makes reduction production process.
For solving above-mentioned technical problem, the technical scheme is that：A kind of production method of n-propyl acetate, its innovation
Point is that described step is：Step S1：Acetic acid and propanol are according to volume ratio 1.3:1 prepares in preheated rear entrance esterification column, leads to
The Matter Transfer heating continuous circulating-heating of passage that over-churning tower and esterification column reboiler are formed, raw material is gasified entrance esterification column
In under catalyst action reaction generate n-propyl acetate, the propanol warp of the n-propyl acetate of generation and water and not reaction completely
Cross condensation and obtain thick n-propyl acetate；Step S2：Treating column sent into by thick n-propyl acetate after being preheated to 75 ~ 80 DEG C, treating column with
The propyl ester circulation rectification passage for the treatment of column reboiler composition, by the internal thick acetic acid of the steam in treating column reboiler heat medium passage
The continuous indirectly heat of n-propyl, the vapor in thick n-propyl acetate, impurity constantly escape formation top gaseous phase thing, leave acetic acid
N-propyl finished product；In the process, the pressure for the treatment of column bottom of towe is made to be maintained at by controlling the steam pressure for the treatment of column reboiler
In the range of 300～350kPa, and the pressure of refined column overhead is maintained in the range of 250～299kPa；Step S3：Step S2
Middle treating column top gaseous phase thing is sent in scalp pomade tank after partial condensation, includes liquid and gas in scalp pomade tank simultaneously：Scalp pomade
In tank, bottom is liquid scalp pomade, and part scalp pomade is pumped to refined column overhead, and another part scalp pomade is then sent into esterification column and added again
Heat；Scalp pomade tank internal upper part is low boiling gaseous component, control scalp pomade pressure tank so that scalp pomade pressure inside the tank be higher than esterification column 30 ~
50kPa, and then low boiling gaseous component is passed directly into by the continuation participation reaction of esterification column bottom by pipeline.
Preferably, described treating column top gaseous phase thing is passed through the heat medium passage of esterification column reboiler and acetic acid and propanol heat are handed over
Change and be condensed.
Preferably, the steam in described treating column reboiler heat medium passage continues on for after thick n-propyl acetate is heated slightly
N-propyl acetate enters the preheating before treating column.
It is an advantage of the current invention that：
1. in scalp pomade tank, some lower boiling compositions continue presented in gas phase at a higher temperature in scalp pomade tank
In, by pressure-regulating valve adjust scalp pomade tank and esterification column pressure reduction between 30 ~ 50kPa so that this is partly lower boiling
Gas gas-phase objects are passed into entrance esterification column to be continued to participate in reaction, provides part of heat energy for reaction simultaneously, can effectively improve product
The yield of product, reduces the energy being lost because low boiling point component circulates in refining system for a long time；Meanwhile, by controlling scalp pomade
The pressure of tank, can make the heating for esterification that treating column gas phase is stable, increased the stable of system and operability.
2. thick ester, before entering treating column, due to having the composition of basic, normal, high different boiling, by way of preheating, makes
Change into the form of gas phase after lower boiling component is preheated, even if high boiling component can not be fully vaporized prior, also can be carried
Rectifying column is entered in the form of liquid phase, scalp pomade also maintains relatively high temperature and flowed back, as appearance simultaneously after rising temperature
Cold material is quenched the situation of gas phase steam.
3. by way of using compression rectification, not only increase the boiling point difference of separated object material different component so that
In the packing layer of same height, the separating effect of different component becomes more preferable.
4. the steam of esterification reboiler is changed to the thermal source of the gas phase for the treatment of column as esterification, greatly reduces steaming
The usage amount of vapour.And propyl ester treating column is no longer necessary to condenser cooling, greatly reduces the usage amount of recirculated water, reduce product
Power consumption.Decrease the equipment of system, reduce the investment in fixed assets of product.
Specific embodiment
Step S1：Acetic acid and propanol are according to volume ratio 1.3:In 1 preheated rear entrance esterification column, 75 ~ 80 DEG C of preheating temperature；
The continuous circulating-heating of passage is heated to 120 DEG C by the Matter Transfer that esterification column and esterification column reboiler are formed, raw material is gasified
Enter in esterification column reaction under catalyst action and generate n-propyl acetate, the n-propyl acetate of generation and water and completely not anti-
The propanol answered obtains thick n-propyl acetate through condensation；
Step S2：Treating column sent into by thick n-propyl acetate after being preheated to 75 ~ 80 DEG C, treating column is formed with treating column reboiler
Propyl ester circulation rectification passage, by the internal thick n-propyl acetate of the steam in treating column reboiler heat medium passage constantly indirectly plus
To 160 ~ 165 DEG C, the vapor in thick n-propyl acetate, impurity constantly escape formation top gaseous phase thing to heat, leave acetic acid positive third
Ester finished product；
In the process, the pressure for the treatment of column bottom of towe is made to be maintained at 300 by controlling the steam pressure for the treatment of column reboiler
In the range of～350kPa, and the pressure of refined column overhead is maintained in the range of 250～299kPa；
And in this step, thick n-propyl acetate is using the steam not being fully utilized in treating column reboiler heat medium passage
Come to preheat.Make to change into the form of gas phase after lower boiling component is preheated in thick propyl ester, even if high boiling component can not
It is fully vaporized prior, also can enter rectifying column in the form of liquid phase after elevated temperature.
Step S3：In step S2, treating column top gaseous phase thing is passed through heat medium passage and acetic acid and the propanol of esterification column reboiler
Heat exchange, acetic acid and propanol are heated, and gas gas-phase objects are sent in scalp pomade tank after being then partly condensed, now, in scalp pomade tank simultaneously
Including liquid and gas：
In scalp pomade tank, bottom is liquid scalp pomade, and part scalp pomade is pumped to refined column overhead, to reduce treating column reboiler
Load, increase treating column column plate separating effect；Another part scalp pomade is then sent into esterification column and is heated again；
Scalp pomade tank internal upper part is low boiling gaseous component, controls scalp pomade pressure tank 200～250kPa so that scalp pomade tank is intrinsic pressure
Power is higher than esterification column 30 ~ 50kPa, and then it is anti-by pipeline, low boiling gaseous component to be passed directly into the continuation participation of esterification column bottom
Should.Make full use of resource, provide part of heat energy for reaction simultaneously, the yield of product can be effectively improved, reduce because low
The energy that boiling component circulates in refining system for a long time and is lost；Simultaneously as by the pressure controlling scalp pomade tank, can make
The stable heating for esterification for the treatment of column gas phase, increased the stable of system and operability.
To produce n-propyl acetate in aforementioned manners, the energy consumption of n-propyl acetate product per ton can be made to decline 40%.
And this method produces the contrast dividing content and finished product during n-propyl acetate product in esterification column overhead each group：
The esterification thick ester content of column overhead：
| Water | Propanol | Propyl ester | Acid |
| ≤5.02 | ≤4.96 | ≥88.96 | ≤0.002 |
Finished product content：
| Water | Propanol | Propyl ester | Acid |
| ≤0.01 | ≤0.0004 | ≥99.90 | ≤0.002 |
Claims (3)
1. a kind of production method of n-propyl acetate is it is characterised in that described step is：
Step S1：Acetic acid and propanol are according to volume ratio 1.3:1 prepares in preheated rear entrance esterification column, by esterification column and esterification
The Matter Transfer heating continuous circulating-heating of passage that tower reboiler is formed, raw material is gasified and is entered in esterification column in catalyst action
Lower reaction generates n-propyl acetate, and the n-propyl acetate of generation obtains thick second with the propanol of water and not reaction completely through condensation
Sour n-propyl；
Step S2：Thick n-propyl acetate sends into treating column, treating column and the third for the treatment of column reboiler composition after being preheated to 75 ~ 80 DEG C
Ester circulates rectification passage, by the internal continuous indirectly heat of thick n-propyl acetate of the steam in treating column reboiler heat medium passage,
Vapor in thick n-propyl acetate, impurity constantly escape formation top gaseous phase thing, leave n-propyl acetate finished product；
In the process, by control the steam pressure for the treatment of column reboiler make the pressure for the treatment of column bottom of towe be maintained at 300～
In the range of 350kPa, and the pressure of refined column overhead is maintained in the range of 250～299kPa；
Step S3：In step S2, treating column top gaseous phase thing is sent in scalp pomade tank after partial condensation, wraps in scalp pomade tank simultaneously
Include liquid and gas：
In scalp pomade tank, bottom is liquid scalp pomade, and part scalp pomade is pumped to refined column overhead, and esterification then sent into by another part scalp pomade
Tower heats again；
Scalp pomade tank internal upper part is low boiling gaseous component, control scalp pomade pressure tank so that scalp pomade pressure inside the tank be higher than esterification column 30 ~
50kPa, and then low boiling gaseous component is passed directly into by the continuation participation reaction of esterification column bottom by pipeline.
2. n-propyl acetate according to claim 1 production method it is characterised in that：Described treating column top gaseous phase thing
It is passed through the heat medium passage of esterification column reboiler and acetic acid and propanol heat exchange are condensed.
3. n-propyl acetate according to claim 1 production method it is characterised in that：Described treating column reboiler heating agent
Steam in passage continues on for the preheating before thick n-propyl acetate enters treating column after thick n-propyl acetate is heated.
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| CN201510436365.3A CN105037147B (en) | 2015-07-23 | 2015-07-23 | A kind of production method of n-propyl acetate |
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| CN201510436365.3A CN105037147B (en) | 2015-07-23 | 2015-07-23 | A kind of production method of n-propyl acetate |
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| CN105037147A CN105037147A (en) | 2015-11-11 |
| CN105037147B true CN105037147B (en) | 2017-03-08 |
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| CN103254068A (en) * | 2013-05-22 | 2013-08-21 | 江门天诚溶剂制品有限公司 | Energy-saving multi-effect distillation process for producing n-butyl acetate |
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Address after: 226200 Changjiang Town, Rugao City, Rugao, Nantong, Jiangsu, No. 6, Xiangjiang Road Co-patentee after: Jiangsu hundred Sichuan high science and technology new materials Limited by Share Ltd Patentee after: Nantong hundred Sichuan new materials Co., Ltd. Co-patentee after: Rugao ran chemical materials Co., Ltd. Address before: 226500 Rugao, Jiangsu City, the Yangtze River town (Rugao port) Shannon Road, No. 6 Co-patentee before: Wuxi Baichuan Chemical Industrial Co., Ltd. Patentee before: Baichuan Chemical (Rugao) Co., Ltd. Co-patentee before: Hundred river chemical industry are sold Rugao company limited |
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