CN104787779B - The ammonia recovery system produced for PHBA and recovery method - Google Patents

The ammonia recovery system produced for PHBA and recovery method Download PDF

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Publication number
CN104787779B
CN104787779B CN201510162257.1A CN201510162257A CN104787779B CN 104787779 B CN104787779 B CN 104787779B CN 201510162257 A CN201510162257 A CN 201510162257A CN 104787779 B CN104787779 B CN 104787779B
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ammonia
packed absorber
pump
air accumulator
phba
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CN104787779A (en
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雷继中
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LIKAI CHIRALITY TECHNOLOGY Co Ltd CHENGDU
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LIKAI CHIRALITY TECHNOLOGY Co Ltd CHENGDU
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Abstract

The invention discloses a kind of ammonia recovery system produced for PHBA, belong to medication chemistry apparatus field, including dry vacuum extraction unit, described dry vacuum extraction unit includes main pump and backing pump, prime delivery side of pump connects air accumulator, and air accumulator connects the first packed absorber, and the first packed absorber connects heat exchanger, heat exchanger connects dense ammonia tank, also includes the second packed absorber and dilute ammonia tank;The invention also discloses a kind of ammonia recovery method produced for PHBA, the present invention uses dry vacuum extraction unit, air accumulator, blower fan, heat exchanger, the combined system of packed absorber to reclaim the ammonia in product aqueous solution, directly obtain the strong aqua ammonia being available for recycling, substantial amounts of energy need not be consumed again weak ammonia is carried out desorbing, decrease equipment investment and operating cost, cost recovery is low, compare traditional way of recycling, cost recovery reduces by more than 40%, significantly improve economic benefit, greatly reduce environmental pollution simultaneously.

Description

The ammonia recovery system produced for PHBA and recovery method
Technical field
The invention belongs to medication chemistry apparatus field, be specifically related to a kind of ammonia recovery system produced for PHBA.
Background technology
Amikacin is the semi-synthetic aminoglycoside antibiotics of the third generation, to S. aureus L-forms, bacillus pyocyaneus, escherichia coli and Bacillus proteus etc. according to there being stronger pharmacological action, has again the advantages such as low ototoxicity, low nephrotoxicity, is one of the antibiotic of China's wide clinical application.(S)-Alpha-hydroxy-γ-N-phthaloylamino butanoic acid (being called for short PHBA) is the important intermediate of synthetic drug amikacin, in PHBA production technology, gamma-butyrolacton ammonolysis and alkali displacement operation need to use substantial amounts of ammonia, the ammonia that wherein participation chemical reaction is consumed only accounts for 10%, and remaining ammonia of 90% is present among product aqueous solution.Recycle the ammonia having neither part nor lot in reaction significant for reduction production cost, minimizing environmental pollution.Due to the restriction of process conditions, can only remove the ammonia in product aqueous solution at low temperatures, traditional handicraft is to be extracted by the ammonia separation in the product water solution containing ammonia out by fine vacuum.But, the vacuum system that traditional handicraft uses is based on the wet vacuum pump such as liquid-ring type, injecting type, and the ammonia of extracting is mixed into as forming a large amount of weak ammonia in the water of working media.Weak ammonia cannot recycle, strong aqua ammonia can only be absorbed into again in absorption tower after being resolved by weak ammonia by desorber to recycle, the cost reclaiming ammonia is the highest, the most often produce the PHBA of 1 kg, only water resource and two costs of energy consumption about 2.28 yuan, wherein energy consumption about 2.25 yuan, energy consumption is high, causes environmental pollution simultaneously.
Summary of the invention
One of goal of the invention of the present invention is: for the problem of above-mentioned existence, it is provided that it is a kind of that equipment investment is few, cost recovery is low, energy consumption is low, technique simple in a low temperature of ammonia recovery system, to solve the problems referred to above.
nullThe technical solution used in the present invention is such that a kind of ammonia recovery system produced for PHBA,Including dry vacuum extraction unit,Described dry vacuum extraction unit includes main pump and the backing pump being connected with described main pump by pipeline,Described prime delivery side of pump is connected by pipeline air accumulator,The outlet of described air accumulator is connected by pipeline the first packed absorber,It is provided with blower fan between described air accumulator and described first packed absorber,The lower end outlet of described first packed absorber connects heat exchanger,The outlet of described heat exchanger connects dense ammonia tank,The outlet of described dense ammonia tank connects the first pump,Described first delivery side of pump is connected by the top of pipeline and the first packed absorber,The top exit of described first packed absorber is connected by pipeline the second packed absorber,The outlet at bottom of described second packed absorber connects dilute ammonia tank,The outlet connection of described dilute ammonia tank has the second pump,Described second delivery side of pump is connected by the top of pipeline and the second packed absorber,The top exit of described second packed absorber is provided with tail gas blow-down pipe.
Technique scheme utilizes dry vacuum extracting that the product aqueous solution after gamma-butyrolacton ammonolysis is carried out low temperature extracting, the ammonia extracted out enters air accumulator, adjust blower fan intake and ensure air accumulator tiny structure and the suitable blast of packed tower, ammonia in air accumulator is extracted out, send into the first packed absorber, in the first packed absorber, ammonia moves from bottom to top, filling surface with from first packing material absorbing column overhead spray and absorbing liquid counter current contacting, the ammonia of more than 90% is absorbed into ammonia;Absorbing liberated heat to be removed by heat exchanger, the ammonia after cooling enters dense ammonia tank again through the first transport pump to packed tower cyclic absorption, until the ammonia concn in dense ammonia tank reaches to meet the technological requirement of gamma-butyrolacton ammonolysis, then with being pumped into workshop use.The ammonia that first packed absorber has not absorbed enters the second packed absorber lower gas entrance the most afterwards from tower top, blast promote under to tower top rise and filling surface with from second packing material absorbing column overhead spray and absorbing liquid counter current contacting, the ammonia of more than 99.5% enters dilute ammonia tank after being absorbed into ammonia, then through the second transport pump to packed tower cyclic absorption.The absorbing liquid of dense ammonia tank is supplemented from dilute ammonia tank, and the absorbing liquid tap water of dilute ammonia tank supplements.
As preferred technical scheme: described main pump is Roots vaccum pump, and it is provided with two Roots vaccum pumps, including one-level Roots vaccum pump and two grades of Roots vaccum pumps.
Technical scheme as further preferred: be additionally provided with heat exchanger between described two grades of Roots vaccum pumps and described backing pump.Owing to the gas after Roots vaccum pump compresses can raise temperature volumetric expansion, increase main pump load, in order to solve this problem, so setting up heat exchanger in lobe pump outlet.
The preferred spiral heat exchanger of above-mentioned heat exchanger, backing pump preferred oil-free reciprocating pump or dry screw vacuum pump, the preferred roots blower of blower fan.
The two of the purpose of the present invention, are to provide a kind of method using said system to carry out recovery ammonia, and the technical scheme of employing is: comprise the following steps:
(1) low temperature extracting: the product aqueous solution after gamma-butyrolacton ammonolysis is carried out low temperature extracting, the ammonia extracted enters air accumulator;
(2) ammonia is inhaled: the ammonia obtained in step (1) is sent into from air accumulator the first packed absorber, ammonia and the absorbing liquid counter current contacting of described first packing material absorbing column overhead, is absorbed into ammonia;Ammonia after cooling enters dense ammonia tank and delivers to the first packed absorber cyclic absorption again, until the ammonia concn in dense ammonia tank reaches to meet the technological requirement of gamma-butyrolacton ammonolysis, is then fed into workshop and uses;Wherein, with tap water being injected the dense ammonia tank absorbing liquid as the first packed absorber when driving first to run, properly functioning after just pump into the weak ammonia absorbing liquid as the first packed absorber from dilute ammonia tank to dense ammonia tank when being supplemented with absorbing liquid.
(3) secondary inhales ammonia: the ammonia that the first packed absorber has not absorbed enters the second packed absorber lower gas entrance the most afterwards from tower top, absorbing liquid counter current contacting with the second packed absorber, absorb into ammonia laggard enter dilute ammonia tank, then through the second transport pump to the second packed absorber cyclic absorption;Wherein, the absorbing liquid of the second packed absorber is to inject the tap water absorbing liquid as the second packed absorber to dilute ammonia tank.
As preferred technical scheme: reservoir pressure is-20~0k Pa(gauge pressures), the admission pressure 2~10kPa(gauge pressure of the first packed absorber), the sprinkle density of the first packed absorber and the second packing material absorbing column overhead is 14~20m3/m2·h.It is regulation roots blower terminal valve that pressure adjusts mode, and sprinkle density regulative mode is regulation packed absorber Cyclic Rings pump discharge valve.The effect that such control can make ammonia absorb is more preferable.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows: the present invention uses dry vacuum extraction unit, air accumulator, blower fan, heat exchanger, the combined system of packed absorber to reclaim the ammonia in product aqueous solution, directly obtain the strong aqua ammonia being available for recycling, substantial amounts of energy need not be consumed again weak ammonia is carried out desorbing, decrease equipment investment and operating cost, cost recovery is low, compare traditional way of recycling, cost recovery reduces by more than 40%, significantly improve economic benefit, greatly reduce environmental pollution simultaneously.
Accompanying drawing explanation
Fig. 1 is the structured flowchart of the embodiment of the present invention 1;
In figure, 1 is one-level Roots vaccum pump, and 2 is two grades of Roots vaccum pumps, and 3 is the first spiral heat exchanger, 4 is oil-free reciprocating pump, 5 is air accumulator, and 6 is roots blower, and 7 is the first packed absorber, 8 is secondary spiral lamina formula heat exchanger, 9 is dense ammonia tank, and 10 is the second packed absorber, and 11 is dilute ammonia tank.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the present invention is described in detail.
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
nullAs shown in Figure 1,In figure, the direction of arrow is liquid/gas flow direction,A kind of ammonia recovery system produced for PHBA,Including dry vacuum extraction unit,Described dry vacuum extraction unit includes main pump and the backing pump being connected with described main pump by pipeline,Described main pump is Roots vaccum pump,And it is provided with two Roots vaccum pumps,Including one-level Roots vaccum pump 1 and two grades of Roots vaccum pumps 2,Described backing pump is oil-free reciprocating pump 4,The first spiral heat exchanger 3 it is additionally provided with between two grades of Roots vaccum pumps 2 and institute's oil-free reciprocating pump 4,It is provided with check valve on pipeline between two grades of Roots vaccum pumps 2 and the first spiral heat exchanger 3,The outlet of oil-free reciprocating pump 4 is connected by pipeline air accumulator 5,It is also equipped with check valve on pipeline between oil-free reciprocating pump 4 and air accumulator 5,The outlet of air accumulator 5 is connected by pipeline the first packed absorber 7,It is provided with roots blower 6 between air accumulator 5 and the first packed absorber 7,The lower end outlet of the first packed absorber 7 connects secondary spiral lamina formula heat exchanger 8,The outlet of secondary spiral lamina formula heat exchanger 8 connects dense ammonia tank 9,The outlet of dense ammonia tank 9 connects the first pump,Described first delivery side of pump is connected by the top of pipeline and the first packed absorber 7,The top exit of the first packed absorber 7 is connected by pipeline the second packed absorber 10,The outlet at bottom of the second packed absorber 10 connects dilute ammonia tank 11,Dilute ammonia tank 11 exports connection the second pump,Described second delivery side of pump is connected by the top of pipeline and the second packed absorber 10,The top exit of the second packed absorber 10 is provided with tail gas blow-down pipe.
Embodiment 2
A kind of ammonia recovery method produced for PHBA, comprises the following steps:
(1) low temperature extracting: the product aqueous solution after gamma-butyrolacton ammonolysis is carried out low temperature extracting, the ammonia extracted enters air accumulator;
(2) ammonia is inhaled: the ammonia obtained in step (1) is sent into from air accumulator the first packed absorber, ammonia and the absorbing liquid counter current contacting of described first packing material absorbing column overhead, is absorbed into ammonia;Ammonia after cooling enters dense ammonia tank and delivers to the first packed absorber cyclic absorption again, until the ammonia concn in dense ammonia tank reaches to meet the technological requirement of gamma-butyrolacton ammonolysis, is then fed into workshop and uses;
(3) secondary inhales ammonia: the ammonia that the first packed absorber has not absorbed enters the second packed absorber lower gas entrance the most afterwards from tower top, absorbing liquid counter current contacting with the second packed absorber, absorb into ammonia laggard enter dilute ammonia tank, then through the second transport pump to the second packed absorber cyclic absorption.
In the present embodiment, reservoir pressure is-10~0k Pa(gauge pressures), the admission pressure 2~10kPa(gauge pressure of the first packed absorber), sprinkle density is 14~20m3/m2·h。
Use said method, often produce the ammonia that the PHBA of 1kg produces, cost recovery only water and energy consumption cost are 1.354 yuan/1kgPHBA, energy consumption is 1.35 yuan/1kgPHBA, compared with conventional art, the water of this method and energy consumption cost can reduce by 0.926 yuan/more than 1kgPHBA, and energy consumption reduces by 0.9 yuan/more than 1kgPHBA.Often producing the ammonia that the PHBA of 1kg produces, the recovery method of the present invention consumes 2.5kg water, and traditional method consumes 20kg water/1kgPHBA, and the water after traditional method desorbing can not realize fully recovering, and the PHBA often producing 1kg needs to environmental emission about 17 Kg waste water, and this method can realize removal process wastewater zero discharge.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.

Claims (5)

  1. null1. the ammonia recovery system produced for PHBA,It is characterized in that: include dry vacuum extraction unit,Described dry vacuum extraction unit includes main pump and the backing pump being connected with described main pump by pipeline,Described prime delivery side of pump is connected by pipeline air accumulator,The outlet of described air accumulator is connected by pipeline the first packed absorber,It is provided with blower fan between described air accumulator and described first packed absorber,The lower end outlet of described first packed absorber connects heat exchanger,The outlet of described heat exchanger connects dense ammonia tank,The outlet of described dense ammonia tank connects the first pump,Described first delivery side of pump is connected by the top of pipeline and the first packed absorber,The top exit of described first packed absorber is connected by pipeline the second packed absorber,The outlet at bottom of described second packed absorber connects dilute ammonia tank,The outlet connection of described dilute ammonia tank has the second pump,Described second delivery side of pump is connected by the top of pipeline and the second packed absorber,The top exit of described second packed absorber is provided with tail gas blow-down pipe.
  2. The ammonia recovery system produced for PHBA the most according to claim 1, it is characterised in that: described main pump is Roots vaccum pump, and is provided with two-stage Roots vaccum pump, including one-level Roots vaccum pump and two grades of Roots vaccum pumps.
  3. The ammonia recovery system produced for PHBA the most according to claim 2, it is characterised in that: it is additionally provided with heat exchanger between described two grades of Roots vaccum pumps and described backing pump.
  4. 4. the recovery system using claim 1 carries out the method for recovery ammonia of PHBA production, it is characterised in that comprise the following steps:
    (1) low temperature extracting: the product aqueous solution after gamma-butyrolacton ammonolysis is carried out low temperature extracting, the ammonia extracted enters air accumulator;
    (2) ammonia is inhaled: the ammonia obtained in step (1) is sent into from air accumulator the first packed absorber, ammonia and the absorbing liquid counter current contacting of described first packing material absorbing column overhead, is absorbed into ammonia;Ammonia after cooling enters dense ammonia tank and delivers to the first packed absorber cyclic absorption again, until the ammonia concn in dense ammonia tank reaches to meet the technological requirement of gamma-butyrolacton ammonolysis, is then fed into workshop and uses;
    (3) secondary inhales ammonia: the ammonia that the first packed absorber has not absorbed enters the second packed absorber lower gas entrance the most afterwards from tower top, absorbing liquid counter current contacting with the second packed absorber, absorb into ammonia laggard enter dilute ammonia tank, then through the second transport pump to the second packed absorber cyclic absorption.
  5. Recovery method the most according to claim 4, it is characterised in that: reservoir pressure is-20~0k Pa, and the first packed absorber inlet pressure is 2~10kPa;The sprinkle density of the first packed absorber and the second packing material absorbing column overhead is 14~20m3/m2·h。
CN201510162257.1A 2015-04-08 2015-04-08 The ammonia recovery system produced for PHBA and recovery method Active CN104787779B (en)

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CN108585165B (en) * 2018-05-07 2020-03-17 西安交通大学 Ammonia recovery system for supercritical water oxidation system and ammonia recovery control method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4215926A (en) * 1976-12-30 1980-08-05 Hoechst Aktiengesellschaft Process for conducting ammonia in a developing apparatus used for developing diazotype copying material
CN102167454A (en) * 2011-03-04 2011-08-31 大连理工大学 Device and method for recovering ammonia during wastewater treatment
CN203021304U (en) * 2012-11-30 2013-06-26 华中药业股份有限公司 System for recovering ammonia in process of vitamin B1 production
CN204529333U (en) * 2015-04-08 2015-08-05 成都丽凯手性技术有限公司 For the ammonia recovery system that PHBA produces

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITMI20072206A1 (en) * 2007-11-21 2009-05-22 Snam Progetti METHOD FOR THE RECOVERY OF AMMONIA FROM A GAS CURRENT IN A PROCESS OF SYNTHESIS OF UREA

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4215926A (en) * 1976-12-30 1980-08-05 Hoechst Aktiengesellschaft Process for conducting ammonia in a developing apparatus used for developing diazotype copying material
CN102167454A (en) * 2011-03-04 2011-08-31 大连理工大学 Device and method for recovering ammonia during wastewater treatment
CN203021304U (en) * 2012-11-30 2013-06-26 华中药业股份有限公司 System for recovering ammonia in process of vitamin B1 production
CN204529333U (en) * 2015-04-08 2015-08-05 成都丽凯手性技术有限公司 For the ammonia recovery system that PHBA produces

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