CN105037147A - Production method for n-propyl acetate - Google Patents
Production method for n-propyl acetate Download PDFInfo
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- CN105037147A CN105037147A CN201510436365.3A CN201510436365A CN105037147A CN 105037147 A CN105037147 A CN 105037147A CN 201510436365 A CN201510436365 A CN 201510436365A CN 105037147 A CN105037147 A CN 105037147A
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- propyl acetate
- tower
- oil tank
- propyl
- hair oil
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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
Abstract
The invention relates to a production method for n-propyl acetate. The production method is characterized by including the steps that acetic acid and propyl alcohol are preheated and then enter an esterification tower to react and generate the n-propyl acetate, and the rough n-propyl acetate is obtained through condensation; the rough n-propyl acetate is preheated and then sent into a refining tower, and an n-propyl acetate finished product is prepared at the bottom of the tower; gas-phase substances on the top of the refining tower are sent into a primary oil tank after being partially condensed, and the liquid phase and the gas phase are included in the primary oil tank at the same time; low-boiling-point gas-phase components are arranged on the upper portion in the primary oil tank, the pressure of the primary oil tank is controlled, and therefore the low-boiling point gas-phase components are directly injected into the lower portion of the esterification tower through a pipeline to continue to be involved in the reaction. Part of heat sources are provided for the reaction, yield of the product can be effectively increased, and energy lost when the low-boiling-point components are circulated in a refining system for a long time is reduced. Meanwhile, by controlling the pressure of the primary oil tank, the gas phase of the refining tower can be stably used for esterification heating, and stability and operability of the system are increased.
Description
Technical field
The present invention relates to a kind of manufacture method of ester, particularly a kind of production method of n-propyl acetate.
Background technology
N-propyl acetate is the acetic ester of the common lower aliphatic alcohols of a class, and Chang Zuowei coating, ink, nitro spray paint, the fine solvent of varnish and various resin, are also applied to essence and flavoring agent industry.
Along with the requirement of energy saving standard is more and more higher, the manufacturing enterprise of n-propyl acetate also more and more pays close attention to the energy consumption decline of n-propyl acetate production process.And the price competition of these conventional products is more and more fierce, this will ask manufacturing enterprise to need the road constantly seeking to reduce production cost, and thus manufacturing enterprise needs the technique continually developing efficient energy-saving more.
In n-propyl acetate product processes traditional at present, raw material propyl ester and acetic acid enter esterification reboiler after the preheating of peroxyacetic acid feed exchanger and propyl alcohol feed exchanger, esterification reboiler makes material gasification to esterification column through steam heating, in esterification column, under catalyst action, reaction generates thick n-propyl acetate, the thick n-propyl acetate of esterification column overhead extraction enters rectifying tower after reboiler heating, containing the gas phase of light constituent from refining overhead extraction, after condenser cooling, enter hair oil tank, bottom treating tower, produce finished product n-propyl acetate.
According to the production technique of above-mentioned traditional n-propyl acetate, there is no the process what heat makes full use of, esterification needs to consume considerable steam, and the energy consumption of esterification moiety will account for 40 ~ 50% of whole products production energy consumption, and the vapor condensation of refining tower top also needs a large amount of recirculated water; Thick ester enters rectifying tower without prior preheating, easily cause the disorder of Mass and heat transfer in tower, pump, also can the partial gas phase of cancellation tower top to the oil phase of trim the top of column without prior preheating, strengthen the load of tower bottom reboiler, cause the reduction of rectifying tower separation efficiency; Some the lower boiling impurity esters formed after the low-boiling point alcohol brought into by raw alcohol and acid esterification circulate along with oil phase always in refining system, small part is only had to reenter reactive system from hair oil, a large portion comes back to treating tower, increases the energy consumption of refining system.
For the deficiency of existing n-propyl acetate production system, be necessary to develop a kind of method that can reduce energy consumption in production process.
Summary 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 some lower-boiling impurities in system in time, and by the coupling of heat, the energy consumption of reduction production process is reduced.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of production method of n-propyl acetate, its innovative point is that described step is: step S1: acetic acid and propyl alcohol enter in esterification column according to volume ratio 1.3:1 preparation after preheating, by the continuous circulating-heating of Matter Transfer heat tunnel that esterification column and esterification column reboiler are formed, raw material is vaporized to enter in esterification column to react under catalyst action and generates n-propyl acetate, and the propyl alcohol of the n-propyl acetate of generation and water and non-complete reaction obtains thick n-propyl acetate through condensation; Step S2: send into treating tower after thick n-propyl acetate is preheated to 75 ~ 80 DEG C, the propyl ester circulation rectifying passage that treating tower and treating tower reboiler form, the thick n-propyl acetate continuous indirect heating internal by the steam in treating tower reboiler heat medium passage, water vapour in thick n-propyl acetate, impurity are constantly overflowed and are formed overhead gas phases, leave n-propyl acetate finished product; In the process, by the vapor pressure controlling treating tower reboiler, the pressure at the bottom for the treatment of tower tower is remained in the scope of 300 ~ 350kPa, and the pressure for the treatment of tower tower top remain in the scope of 250 ~ 299kPa; Step S3: in step S2, treating tower overhead gas phases is sent in hair oil tank after partial condensation, comprise liquid and gas: in hair oil tank, bottom is liquid hair oil in hair oil tank simultaneously, part hair oil is pumped to treating tower tower top, and another part hair oil is then sent into esterification column and again heated; Hair oil tank internal upper part is lower boiling gaseous component, control head tank pressure, makes hair oil tank internal pressure higher than esterification column 30 ~ 50kPa, and then by pipeline, lower boiling gaseous component is directly passed into the continuation participation reaction of esterification column bottom.
Preferably, described treating tower overhead gas phases passes into the heat medium passage of esterification column reboiler and acetic acid and propyl alcohol heat exchange and is condensed.
Preferably, the steam in described treating tower reboiler heat medium passage enters the preheating before treating tower to continuing on for thick n-propyl acetate after thick n-propyl acetate heating.
The invention has the advantages that:
1. in hair oil tank, some lower boiling compositions continue to be present in hair oil tank with the form of gas phase at a higher temperature, by pressure regulator valve adjusting head oil tank and esterification column pressure reduction between 30 ~ 50kPa, the lower boiling gas gas-phase objects of this part is passed into and enters esterification column continuation participation reaction, simultaneously for reaction provides part of heat energy, effectively can improve the yield of product, reduce because low boiling point component circulates and the energy of loss for a long time in refining system; Meanwhile, by the pressure of control head oil tank, the heating for esterification that treating tower gas phase is stable can be made, add the stable of system and operability.
2. thick ester is before entering treating tower, owing to having the composition of basic, normal, high different boiling, by the mode of preheating, make lower boiling component after preheating, change into the form of gas phase, even if high boiling component can not be fully vaporized prior, also can be entered rectifying tower by after lifting temperature with the form of liquid phase, simultaneously hair oil also maintains relatively high temperature and refluxes, as the situation occurring cold material cancellation gas phase steam.
3. by adopting the mode of compression rectification, not only increase the boiling point difference of separated material different components, make in the packing layer of same height, the separating effect of different components becomes better.
4. the steam of esterification reboiler is changed into the thermal source of gas phase as esterification for the treatment of tower, greatly reduce the usage quantity of steam.And propyl ester treating tower no longer needs condenser to cool, greatly reduce the usage quantity of recirculated water, reduce the power consumption of product.Decrease the equipment of system, reduce the investment in fixed assets of product.
Embodiment
Step S1: acetic acid and propyl alcohol enter in esterification column according to volume ratio 1.3:1 after preheating, preheating temperature 75 ~ 80 DEG C; By the continuous circulating-heating to 120 DEG C of Matter Transfer heat tunnel that esterification column and esterification column reboiler are formed, raw material is vaporized to enter in esterification column to react under catalyst action and generates n-propyl acetate, and the propyl alcohol of the n-propyl acetate of generation and water and non-complete reaction obtains thick n-propyl acetate through condensation;
Step S2: send into treating tower after thick n-propyl acetate is preheated to 75 ~ 80 DEG C, the propyl ester circulation rectifying passage that treating tower and treating tower reboiler form, thick n-propyl acetate continuous indirect heating to 160 ~ 165 DEG C internal by the steam in treating tower reboiler heat medium passage, water vapour in thick n-propyl acetate, impurity are constantly overflowed and are formed overhead gas phases, leave n-propyl acetate finished product;
In the process, by the vapor pressure controlling treating tower reboiler, the pressure at the bottom for the treatment of tower tower is remained in the scope of 300 ~ 350kPa, and the pressure for the treatment of tower tower top remain in the scope of 250 ~ 299kPa;
And in this step, thick n-propyl acetate adopts the steam be not fully utilized in treating tower reboiler heat medium passage to carry out preheating.Make lower boiling component in thick propyl ester after preheating, change into the form of gas phase, even if high boiling component can not be fully vaporized prior, also can be entered rectifying tower by after lifting temperature with the form of liquid phase.
Step S3: in step S2, treating tower overhead gas phases passes into the heat medium passage of esterification column reboiler and acetic acid and propyl alcohol heat exchange, acetic acid and propyl alcohol are heated, gas gas-phase objects is then partly condensed in rear feeding hair oil tank, now, comprises liquid and gas in hair oil tank simultaneously:
In hair oil tank, bottom is liquid hair oil, and part hair oil is pumped to treating tower tower top, to reduce the load for the treatment of tower reboiler, increases the separating effect for the treatment of tower column plate; Another part hair oil is then sent into esterification column and is again heated;
Hair oil tank internal upper part is lower boiling gaseous component, control head tank pressure 200 ~ 250kPa, makes hair oil tank internal pressure higher than esterification column 30 ~ 50kPa, and then by pipeline, lower boiling gaseous component is directly passed into the continuation participation reaction of esterification column bottom.Make full use of resource, simultaneously for reaction provides part of heat energy, effectively can improve the yield of product, reduce because low boiling point component circulates and the energy of loss for a long time in refining system; Meanwhile, due to the pressure by control head oil tank, the heating for esterification that treating tower gas phase is stable can be made, add the stable of system and operability.
Produce n-propyl acetate with aforesaid method, the energy consumption of n-propyl acetate product per ton can be made to decline 40%.
And present method when producing n-propyl acetate product in the contrast of each component concentration of esterification column tower top and finished product:
The thick ester content of esterification column tower top:
| Water | Propyl alcohol | Propyl ester | Acid |
| ≤5.02 | ≤4.96 | ≥88.96 | ≤0.002 |
Finished product content:
| Water | Propyl alcohol | Propyl ester | Acid |
| ≤0.01 | ≤0.0004 | ≥99.90 | ≤0.002 |
Claims (3)
1. a production method for n-propyl acetate, is characterized in that described step is:
Step S1: acetic acid and propyl alcohol enter in esterification column according to volume ratio 1.3:1 preparation after preheating, by the continuous circulating-heating of Matter Transfer heat tunnel that esterification column and esterification column reboiler are formed, raw material is vaporized to enter in esterification column to react under catalyst action and generates n-propyl acetate, and the propyl alcohol of the n-propyl acetate of generation and water and non-complete reaction obtains thick n-propyl acetate through condensation;
Step S2: send into treating tower after thick n-propyl acetate is preheated to 75 ~ 80 DEG C, the propyl ester circulation rectifying passage that treating tower and treating tower reboiler form, the thick n-propyl acetate continuous indirect heating internal by the steam in treating tower reboiler heat medium passage, water vapour in thick n-propyl acetate, impurity are constantly overflowed and are formed overhead gas phases, leave n-propyl acetate finished product;
In the process, by the vapor pressure controlling treating tower reboiler, the pressure at the bottom for the treatment of tower tower is remained in the scope of 300 ~ 350kPa, and the pressure for the treatment of tower tower top remain in the scope of 250 ~ 299kPa;
Step S3: in step S2, treating tower overhead gas phases is sent in hair oil tank after partial condensation, comprises liquid and gas in hair oil tank simultaneously:
In hair oil tank, bottom is liquid hair oil, and part hair oil is pumped to treating tower tower top, and another part hair oil is then sent into esterification column and again heated;
Hair oil tank internal upper part is lower boiling gaseous component, control head tank pressure, makes hair oil tank internal pressure higher than esterification column 30 ~ 50kPa, and then by pipeline, lower boiling gaseous component is directly passed into the continuation participation reaction of esterification column bottom.
2. the production method of n-propyl acetate according to claim 1, is characterized in that: described treating tower overhead gas phases passes into the heat medium passage of esterification column reboiler and acetic acid and propyl alcohol heat exchange and is condensed.
3. the production method of n-propyl acetate according to claim 1, is characterized in that: the steam in described treating tower reboiler heat medium passage enters the preheating before treating tower to continuing on for thick n-propyl acetate after thick n-propyl acetate heating.
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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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| CN105037147B CN105037147B (en) | 2017-03-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943840A (en) * | 2020-07-27 | 2020-11-17 | 浙江建业化工股份有限公司 | Treatment process of n-propyl acetate bed charge |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
| 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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2015
- 2015-07-23 CN CN201510436365.3A patent/CN105037147B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 王冰旭等: "乙酸正丙酯装置回流工艺的优化与生产成本核算", 《南京工业大学学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943840A (en) * | 2020-07-27 | 2020-11-17 | 浙江建业化工股份有限公司 | Treatment process of n-propyl acetate bed charge |
| CN111943840B (en) * | 2020-07-27 | 2022-08-23 | 浙江建业化工股份有限公司 | Treatment process of n-propyl acetate bed charge |
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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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