CN104383702A - Organic acid purifying method and its apparatus - Google Patents
Organic acid purifying method and its apparatus Download PDFInfo
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- CN104383702A CN104383702A CN201410546349.5A CN201410546349A CN104383702A CN 104383702 A CN104383702 A CN 104383702A CN 201410546349 A CN201410546349 A CN 201410546349A CN 104383702 A CN104383702 A CN 104383702A
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Abstract
The invention relates to the technical field of production of organic acids and derivatives thereof, and discloses an organic acid purifying method and its apparatus. The method comprises the following steps: inputting a crude organic acid into a falling film evaporator, and evaporating; and introducing a gas and liquid mixture obtained after evaporation into a gas-liquid separation tank, separating to obtain an organic acid gas with the purity of above 99.9% and a liquid phase product, returning parts of the liquid phase product to the falling film evaporator in order to carry out cycle evaporation, and carrying out tailing collection on the remaining liquid phase product. The organic acid purifying method avoids the disadvantages of high temperature and easy polymerization of traditional rectification purifying methods, and has the advantages of low material evaporation temperature, short heating time, high separation degree and low separation cost. The organic acid purifying apparatus comprises the falling film evaporator, the gas-liquid separation tank, a liquid phase circulating pump and a liquid phase discharging pump. The purifying apparatus has the advantages of reasonable and compact structure, small device investment, low cost, and suitableness for being applied in the field of the organic acid purifying industry.
Description
Technical field
The present invention relates to the production technical field of organic acid and derivative thereof, particularly a kind of method of purification of organic acid and device thereof.
Background technology
Organic acid, it is as the intermediate of important Organic Chemicals and polymer, the height of its product purity directly has larger impact to the quality of follow-up sintetics, and the current separation method of organic acid usually adopts rectifying and extraction separating method, because its rectifying separating pressure, temperature are high, investment is large, and separating energy consumption is high, inefficiency, and with self-polymeric reaction, exist equipment investment costly, the shortcoming of complex process, be difficult to obtain high purity product by traditional rectificating method, and affect the purity of product, also have impact on the economic benefit of enterprise; And chemical extraction method brings new pollution, eliminate old impurity often and bring again new impurity, this chemical method removes impurity in organic acid, by adding aldehyde in a small amount of chemical reagent and organic acid acid or other react and carry out imurity-removal, this method imurity-removal is limited in one's ability, and can solid residue be produced in subtractive process, obtained organic acid still difficulty meets high-purity organic acid Production requirement, is difficult to heavy industrialization and uses.In China under the energy-saving and environmental protection of commercial plant, the efficient background required, development of new energy-saving and environmental protection, organic acid separation method is very important and urgent efficiently.
The separation chamber's major function carried in falling film evaporator in prior art is gas-liquid separation, but the scope of application is narrower, for the operating mode that gas phase flow rate is larger, is difficult to realize effective gas-liquid separation.The falling film evaporator difference with the prior art that embodiments of the present invention provide is, falling film evaporator is without the separation chamber carried, but adopt external knockout drum, gas-liquid two-phase is separated in knockout drum, liquid phase obtains sedimentation and comes together in tank base and keep certain liquid level, high-purity gaseous products is then discharged by from tank body top, achieves the gas-liquid separation in the larger situation of air-flow.
Preferably, knockout drum is vertical tank body, and the middle part of knockout drum is located in its input port, ensure that the realization of gas liquid separating function in knockout drum.Gas-fluid two-phase mixture enters tank body from the middle part of knockout drum, and gas phase flow velocity is less than the floating flow velocity of hanging drop, and liquid phase obtains sedimentation and comes together in tank base and keep certain liquid level, and high-purity gaseous products is from the extraction of tank body top.
The purifying organic acid apparatus structure that embodiments of the present invention provide rationally compact, equipment investment is little, be conducive to reduce purifying organic acid operation cost, be suitable for the application of purifying organic acid industrial circle.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of method utilizing falling film evaporator purification of organic acid, to overcome traditional rectification and purification method and chemical extraction temperature in purification process is high, organic acid molecule is easily polymerized, production cost is high shortcoming.
The device that the present invention also provides the method for this kind of purification of organic acid special simultaneously.
For solving the problems of the technologies described above, the method for purification of organic acid provided by the present invention, comprises following steps:
Crude product organic acid input falling film evaporator is evaporated, generates gas-liquid mixture;
Be separated by knockout drum by the above-mentioned gas-liquid mixture obtaining abundant mass exchange, obtain gaseous products and liquid-phase product respectively, described gaseous products is the high-purity organic acid gas of purifying and obtaining; A described liquid-phase product part returns falling film evaporator and carries out circulating and evaporating, and remainder is collected as tailing;
Describedly return 4 ~ 7 times that amount that falling film evaporator carries out the liquid-phase product of circulating and evaporating is the crude product organic acid liquid supply rate of described input falling film evaporator.
In purifying organic acid method of the present invention, certain density crude product organic acid enters falling film evaporator and evaporates, organic acid due to boiling point lower, organic acid heats rapidly by the heat exchange efficiency higher by falling film evaporator and larger heat exchange area, makes it be evaporated to gaseous state; Heavy constituent is then because boiling point is more high-leveled and difficult with evaporation, still keep liquid phase state, mixture sufficient molecule in falling film evaporator of the organic acid of gaseous state obtained above and the heavy component of liquid phase exchanges, namely in gas mixture, impurity is dissolved in liquid phase again, thus the impurity content reduced in gas, and the organic acid in liquid phase evaporates again, improve organic acid evaporation capacity, obtain the organic acid gas of abundant mass exchange and the gas-liquid mixture of heavies liquid composition thus.
The above-mentioned gas-liquid mixture obtaining abundant mass exchange is after falling film evaporator flows out, enter next stage knockout drum to be separated, in knockout drum, gas phase flow velocity is less than the floating flow velocity of hanging drop, liquid phase generation sedimentation and come together in the tank base of knockout drum and keep certain liquid level, gaseous products is from the extraction of tank body top, and this gaseous products is the present invention and purifies the high-purity organic acid gas obtained; A part in liquid-phase product (heavy constituent namely in organic acid crude product and a small amount of organic acid) returns falling film evaporator and carries out circulating-heating, and remaining liquid-phase product is then collected as tailing.Wherein, above-mentionedly return 4 ~ 7 times that amount that falling film evaporator carries out the liquid-phase product of circulating and evaporating is the crude product organic acid liquid supply rate of input falling film evaporator, this part is evaporated again for organic acid residual in the liquid phase of circulating and evaporating, by the control of the internal circulating load to circulating and evaporating liquid-phase product, namely control the mass exchange time of the rear gas of evaporation and liquid, highly purified organic acid gas is adopted to obtain in gas-liquid separation tank top.
In terms of existing technologies, the method of purification of organic acid provided by the present invention, by falling film evaporator and knockout drum with the use of, without the need to adding other chemical reagent, the impurity in organic acid is removed, also without the need to adding polymerization inhibitor, solve chemical method and remove the problem that in organic acid, impurity purity is not high, avoid the problem of easily polymerization, purity instability in purifying organic acid process simultaneously.The method of purification of organic acid of the present invention, have operating temperature low, purify obtain the feature that product purity is high, polymerization activity is high.
In the method for the purification of organic acid that embodiments of the present invention provide, crude product organic acid purity in order to purify is 90% ~ 99%, the organic acid of aliphatic acid, sulfonic acid and aromatic series kind is all generally suitable for method provided by the present invention and purifies, for example, the crude product organic acid kind of purifying for the present invention can be formic acid, acetic acid, propionic acid, acrylic acid aliphatic acid or benzoic acid.
Preferably, in the method for the purification of organic acid that embodiments of the present invention provide, when falling film evaporator evaporates crude product organic acid, temperature is 30 ~ 120 DEG C, and pressure is 0 ~ 100kPa; Falling film evaporator is made to be 10 ~ 35% to the rate of gasification that crude product organic acid evaporates.
Preferably, in the method for the purification of organic acid that embodiments of the present invention provide, when knockout drum is separated gas-liquid mixture, temperature is 30 ~ 120 DEG C, and pressure is 0 ~ 100kPa.
Preferably, in the method for the purification of organic acid that embodiments of the present invention provide, the amount as the liquid-phase product of tailing collection is less than 15% of described crude product organic acid liquid supply rate.
Embodiments of the present invention additionally provide the special purpose device of the method being applicable to above-mentioned purification of organic acid, this device comprises falling film evaporator, knockout drum, liquid phase circulation pump and liquid phase discharging pump, the top of this falling film evaporator is provided with charging aperture, inputs for crude product organic acid; The bottom of falling film evaporator is provided with discharging opening, exports for gas-liquid mixture; The discharging opening of falling film evaporator is connected with the input port of knockout drum, and the top of knockout drum is provided with gas phase acquisition port, for gaseous products collection; The bottom of knockout drum is connected with liquid phase discharging pump with liquid phase circulation pump respectively; Liquid phase circulation pump is connected with the charging aperture of falling film evaporator by circulation line, and pass through for returning the liquid-phase product that falling film evaporator carries out circulating and evaporating, liquid phase discharging pump is provided with tailing outlet, collects for tailing.Wherein, in the device of the purification of organic acid that embodiments of the present invention provide, the inside of falling film evaporator is provided with connected filming device and heating electrodes pipe.
When the charging aperture of crude product organic acid through being located at falling film evaporator top enter falling film evaporator evaporate time, the filming device (also can be described as distributor) first through falling film evaporator flows into heating tubulation Guan Zhen, heats at the even cloth film of inside pipe wall.Organic acid is lower due to boiling point, is gas through tubulation heating evaporation; And heavy constituent is difficult to evaporation because boiling point is higher on heating tubulation, still keep liquid phase to flow through heating tube, the discharging opening of gas-liquid mixture bottom falling film evaporator of organic acid gas and heavies liquid flows out, and enters the input port of next stage knockout drum.Organic acid gas in knockout drum is gathered by the gas phase acquisition port being located at gas-liquid separation tank top as product, obtains high-purity organic acid gas.Liquid-phase product is then flowed out by the bottom of knockout drum, and a part of liquid-phase product, successively through liquid phase circulation pump and circulation line, is delivered to the charging aperture of falling film evaporator, again carries out circulating-heating, and organic acid residual in liquid phase is evaporated again; The liquid-phase product of remainder is delivered to tailing outlet through liquid phase discharging pump, collects as tailing.
Accompanying drawing explanation
Fig. 1 is the process chart of the method for the purification of organic acid that embodiments of the present invention provide;
Fig. 2 is structural representation and the flow direction of material figure of the device of the purification of organic acid that embodiments of the present invention provide;
Wherein, (1) is falling film evaporator; (2) be knockout drum; (3) be liquid phase circulation pump; (4) be liquid phase discharging pump; (5) be circulation line.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the embodiments of the present invention are explained in detail.But, persons of ordinary skill in the art may appreciate that in each embodiment of the present invention, proposing many ins and outs to make reader understand the application better.But, even without these ins and outs with based on the many variations of following embodiment and amendment, each claim of the application technical scheme required for protection also can be realized.
Embodiment 1
Purity is that the metering system acid crude of 98.5% is with the charging aperture input falling film evaporator 1 of the flow of 5000kg/h through falling film evaporator 1, it is 61 DEG C in temperature, pressure is evaporate under 1.5kPa condition, and the methacrylic acid feed liquid vaporization rate after falling film evaporator 1 processes is 11.5%; The discharging opening of gas-liquid mixture bottom falling film evaporator 1 of gained flows out, and input knockout drum by the input port of knockout drum 2, carry out gas-liquid separation, it is 60.8 DEG C that the operating condition of knockout drum controls in temperature, and pressure is 1.4kPa; The separating obtained gas phase of knockout drum is the metering system acid gas of purity 99.9%, by the gas phase acquisition port extraction at knockout drum 2 top; The separating obtained liquid phase of knockout drum 2 divides two parts to process: a part returns falling film evaporator 1 via liquid phase circulation pump 3 and circulation line 5 successively and carries out circulating and evaporating, and internal circulating load is metering system acid crude liquid supply rate 7 times, i.e. 35000kg/h; Another part is delivered to tailing outlet via liquid phase discharging pump 4, carries out tailing collection, and the amount that tailing is collected is 9.8%, i.e. 492kg/h of metering system acid crude liquid supply rate.
Embodiment 2
Purity is that the acetic acid crude product of 98.8% is with the charging aperture input falling film evaporator 1 of the flow of 4000kg/h through falling film evaporator 1, it is 100 DEG C in temperature, pressure is evaporate under 15kPa condition, and the acetic acid feed liquid vaporization rate after falling film evaporator 1 processes is 12.0%; The discharging opening of gas-liquid mixture bottom falling film evaporator 1 of gained flows out, and input knockout drum by the input port of knockout drum 2, carry out gas-liquid separation, it is 100 DEG C that the operating condition of knockout drum controls in temperature, and pressure is 15kPa; The separating obtained gas phase of knockout drum is the acetic acid gas of purity 99.9%, by the gas phase acquisition port extraction at knockout drum 2 top; The separating obtained liquid phase of knockout drum 2 divides two parts to process: a part returns falling film evaporator 1 via liquid phase circulation pump 3 and circulation line 5 successively and carries out circulating and evaporating, and internal circulating load is acetic acid crude product liquid supply rate 6.2 times, i.e. 24850kg/h; Another part is delivered to tailing outlet via liquid phase discharging pump 4, carries out tailing collection, and the amount that tailing is collected is 12.0%, i.e. 486kg/h of acetic acid acid crude liquid supply rate.
Embodiment 3
Purity be 98% formic acid crude product with the flow of 3500kg/h through falling film evaporator 1 charging aperture input falling film evaporator 1, be 86 DEG C in temperature, pressure is evaporate under 10kPa condition, through falling film evaporator 1 process after acid adding feed liquid vaporization rate be 18.0%; The discharging opening of gas-liquid mixture bottom falling film evaporator 1 of gained flows out, and input knockout drum by the input port of knockout drum 2, carry out gas-liquid separation, it is 86 DEG C that the operating condition of knockout drum controls in temperature, and pressure is 10kPa; The separating obtained gas phase of knockout drum is the formic acid gas of purity 99.8%, by the gas phase acquisition port extraction at knockout drum 2 top; The separating obtained liquid phase of knockout drum 2 divides two parts to process: a part returns falling film evaporator 1 via liquid phase circulation pump 3 and circulation line 5 successively and carries out circulating and evaporating, and internal circulating load is formic acid crude product liquid supply rate 4 times, i.e. 14000kg/h; Another part is delivered to tailing outlet via liquid phase discharging pump 4, carries out tailing collection, and the amount that tailing is collected is 10.0%, i.e. 350kg/h of formic acid crude product liquid supply rate.
Embodiment 4
For the device of purification of organic acid in above-described embodiment 1 ~ 4, comprise falling film evaporator 1, knockout drum 2, liquid phase circulation pump 3 and liquid phase discharging pump 4, the top of falling film evaporator 1 is provided with charging aperture, inputs for crude product organic acid; The inside of falling film evaporator 1 is provided with the filming device and heating electrodes pipe that are connected; The bottom of falling film evaporator 1 is provided with discharging opening, exports for gas-liquid mixture; The discharging opening of falling film evaporator 1 is connected with the input port of knockout drum 2, and knockout drum 2 is vertical tank body, and the middle part of knockout drum 2 is located in input port; The top of knockout drum 2 is provided with gas phase acquisition port, for gaseous products collection; The bottom of knockout drum 2 is connected with liquid phase discharging pump 4 with liquid phase circulation pump 3 respectively; Liquid phase circulation pump 3 is connected by the charging aperture of circulation line 5 with falling film evaporator 1, and pass through for returning the liquid-phase product that falling film evaporator carries out circulating and evaporating, liquid phase discharging pump 4 is provided with tailing outlet, collects for tailing.
When the charging aperture of crude product organic acid through being located at falling film evaporator top enter falling film evaporator evaporate time, the filming device (also can be described as distributor) first through falling film evaporator flows into heating tubulation Guan Zhen, heats at the even cloth film of inside pipe wall.Organic acid is lower due to boiling point, is gas through tubulation heating evaporation; And heavy constituent is difficult to evaporation because boiling point is higher on heating tubulation, still keep liquid phase to flow through heating tube, the discharging opening of gas-liquid mixture bottom falling film evaporator of organic acid gas and heavies liquid flows out, and enters the input port of next stage knockout drum.Knockout drum is vertical tank body, and the middle part of knockout drum is located in its input port, ensure that the realization of gas liquid separating function in knockout drum.Gas-fluid two-phase mixture enters tank body from the middle part of knockout drum, and gas phase flow velocity is less than the floating flow velocity of hanging drop, and liquid phase obtains sedimentation and comes together in tank base and keep certain liquid level, and high-purity gaseous products is from the extraction of tank body top.Liquid-phase product is then flowed out by the bottom of knockout drum, and a part of liquid-phase product, successively through liquid phase circulation pump and circulation line, is delivered to the charging aperture of falling film evaporator, again carries out circulating-heating, and organic acid residual in liquid phase is evaporated again; The liquid-phase product of remainder is delivered to tailing outlet through liquid phase discharging pump, collects as tailing.
Persons of ordinary skill in the art may appreciate that the respective embodiments described above realize specific embodiments of the invention, and in actual applications, various change can be done to it in the form and details, and without departing from the spirit and scope of the present invention.
Claims (9)
1. a method for purification of organic acid, is characterized in that, comprises following steps:
Crude product organic acid input falling film evaporator is evaporated, generates gas-liquid mixture;
Be separated by knockout drum by gas-liquid mixture obtained above, obtain gaseous products and liquid-phase product respectively, described gaseous products is the high-purity organic acid gas of purifying and obtaining; A described liquid-phase product part returns falling film evaporator and carries out circulating and evaporating, and remainder is collected as tailing;
Describedly return 4 ~ 7 times that amount that falling film evaporator carries out the liquid-phase product of circulating and evaporating is the crude product organic acid liquid supply rate of described input falling film evaporator.
2. the method for purification of organic acid according to claim 1, is characterized in that, described crude product organic acid purity is 90% ~ 99%.
3. the method for purification of organic acid according to claim 1, is characterized in that, described crude product organic acid is formic acid, acetic acid, propionic acid, acrylic acid aliphatic acid or benzoic acid.
4. the method for purification of organic acid according to claim 1, is characterized in that, when described falling film evaporator evaporates crude product organic acid, temperature is 30 ~ 120 DEG C, and pressure is 0 ~ 100kPa.
5. the method for purification of organic acid according to claim 1, is characterized in that, when described knockout drum is separated gas-liquid mixture, temperature is 30 ~ 120 DEG C, and pressure is 0 ~ 100kPa.
6. the method for purification of organic acid according to claim 1, is characterized in that, the amount of the described liquid-phase product as tailing collection is less than 15% of described crude product organic acid liquid supply rate.
7. a device for purification of organic acid, is characterized in that, comprises falling film evaporator (1), knockout drum (2), liquid phase circulation pump (3) and liquid phase discharging pump (4),
The top of described falling film evaporator (1) is provided with charging aperture, inputs for crude product organic acid; The bottom of described falling film evaporator (1) is provided with discharging opening, exports for gas-liquid mixture;
The discharging opening of described falling film evaporator (1) is connected with the input port of described knockout drum (2), and the top of described knockout drum (2) is provided with gas phase acquisition port, for gaseous products collection; The bottom of described knockout drum (2) is connected with liquid phase discharging pump (4) with liquid phase circulation pump (3) respectively;
Described liquid phase circulation pump (3) is connected by the charging aperture of circulation line (5) with falling film evaporator (1), pass through for returning the liquid-phase product that falling film evaporator carries out circulating and evaporating, described liquid phase discharging pump (4) is provided with tailing outlet, collects for tailing.
8. the device of purification of organic acid according to claim 7, is characterized in that, the inside of described falling film evaporator (1) is provided with the filming device and heating electrodes pipe that are connected.
9. the device of purification of organic acid according to claim 7, is characterized in that, described knockout drum (2) is vertical tank body, and the middle part of knockout drum (2) is located in described input port.
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| CN201410546349.5A CN104383702A (en) | 2014-10-15 | 2014-10-15 | Organic acid purifying method and its apparatus |
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Cited By (1)
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| CN106810448A (en) * | 2017-01-10 | 2017-06-09 | 中国科学院过程工程研究所 | The processing system and processing method and purposes of waste liquid are produced in a kind of carbonyl synthesis acetic acid |
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| CN103007560A (en) * | 2011-09-26 | 2013-04-03 | 沈阳铝镁设计研究院有限公司 | Configuration structure of last-effect falling-film evaporator and water cooler |
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