CN103351321B - The continuous production method of a kind of NMP - Google Patents

The continuous production method of a kind of NMP Download PDF

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CN103351321B
CN103351321B CN201310245852.2A CN201310245852A CN103351321B CN 103351321 B CN103351321 B CN 103351321B CN 201310245852 A CN201310245852 A CN 201310245852A CN 103351321 B CN103351321 B CN 103351321B
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nmp
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gbl
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CN103351321A (en
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吴兴龙
徐宜彬
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BINZHOU YUNENG CHEMICAL Co Ltd
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Abstract

The invention belongs to the technical field of N-Methyl pyrrolidone manufacture, especially for butyleneglycol prepares the continuous production method of GBL/NMP, be specially a kind of NMP(N-methyl-2-pyrrolidone) continuous energy-saving production method.Technique of the present invention only has lactone and Wan Tongliangge workshop section, the pressure reduction of material qualified in negative pressure tower by existing between two towers, directly from negative pressure tower to rectifying tower punishment in advance, operation is energy-efficient, and whole technologist's proportioning is few, level of automation is high, unit consumption is low, good product quality, output are high.

Description

The continuous production method of a kind of NMP
Technical field
The invention belongs to the technical field of N-Methyl pyrrolidone manufacture, especially for butyleneglycol prepares the continuous production method of GBL/NMP, be specially a kind of NMP(N-methyl-2-pyrrolidone) continuous energy-saving production method.
Background technology
GBL tar chemical name gamma-butyrolactone (GBL).
Gamma-butyrolactone (GBL) is a kind of important Organic Chemicals and fine-chemical intermediate, also be that a kind of functional, solvability is strong, good electrical property, stability are high, nontoxic, the high boiling solvent of use safety, have a wide range of applications in fields such as petrochemical complex, medicine, agricultural chemicals.In the present invention, gamma-butyrolactone produces N-Methyl pyrrolidone (NMP) mainly as intermediate.
NMP chemical name is N-Methyl pyrrolidone (NMP).
N-Methyl pyrrolidone (NMP) is the fine solvent of a kind of high boiling point, environment-friendly type, has viscosity low, chemical stability and Heat stability is good, and polarity is high, and volatility is low, can with water and the advantage such as many organic solvents are infinitely miscible.N-Methyl pyrrolidone market Application Areas mainly concentrates on the industries such as lithium cell, wiring board, insulating material, petrochemical industry, medicine, agricultural chemicals, cleaning, polymer.
Current technique entire work flow is divided into multiple workshop section, for intermittence is produced.Personnel's proportioning is high, and energy consumption is high, product production and quality low.Be all the monomethylamine aqueous solution production NMP of GBL and 40% in the reaction, produce a lot of waste water like this, and heat exhaustion is large, the waste water that reaction produces cannot be recycled, and causes wastage of material and environmental pollution.Wherein, the rectifying of GBL crude product adopted batch-type system in the past, rectifying was divided into Liang Ge workshop section to complete, i.e. negative pressure workshop section, rectification section.Negative pressure workshop section: crude product is fed to negative pressure tower, after taking off low boiling, dry product blanking is to dry product tank.Rectification section: dry product from dry product tank by pump squeeze into rectifying tower more de-height boil.
Have use for laboratory GBL and Monomethylamine sterling to produce the report of NMP, because Monomethylamine sterling flash-point is low, belong to inflammable explosive article, and reaction is a pyroprocess, this method security is not high yet.NMP has aquatic products to go out in generating, and produce a large amount of waste water containing Monomethylamine, and this method cannot reclaim these waste water, causes the waste of raw material, and require higher in sewage disposal after reaction.
Summary of the invention
Object of the present invention provides a kind of NMP(N-methyl-2-pyrrolidone for current Problems existing exactly) continuous production method.
Technical scheme of the present invention is:
A continuous production method of NMP, comprises lactone workshop section and Wan Tong workshop section, and its step is, wherein said lactone workshop section is: after butyleneglycol preheating with heating after hydrogen enter vaporizer in the same way, hydrogen alcohol mol ratio 10:1-5:1; Butyleneglycol enters superheater after vaporizing completely, then enters reactor reaction under copper-based catalysts exists, the temperature 220-250 DEG C of reactor, pressure: 0.06-0.09Mpa; The butyrolactone generated and the gas mixture of hydrogen first by interchanger, then are cooled to 40-80 DEG C after entering condenser condenses, enter GBL crude product tank; Non-condensable gas delivers to hydrogen recycle; Butyrolactone in crude product tank by be pumped to negative pressure tower take off low boil and water obtain dry product GBL, dry product GBL is taken off after height boils by vacuum suction rectifying tower after condensation, delivers to GBL fine work tank;
Described Wan Tong workshop section is: GBL fine work and mass concentration are enter alkane reactive ketone bed after 40% Monomethylamine solution mixes, under high-temperature and high-pressure conditions, fully reaction produces NMP crude product, wherein temperature of reaction is 265-285 DEG C, reaction pressure is 6.5-8.0MPa, the NMP crude product obtained enters atmospheric tower flash distillation again and to anhydrate point and Monomethylamine, semi-dried product is become to enter NMP crude product tank, Monomethylamine and moisture are discharged after the laggard methylamine withdrawing can of condensation by being pumped to the process of methylamine decomposition tower by tower top, described methylamine is reused for and participates in reaction, semi-dried product NMP is by being pumped to negative pressure tower, de-lowly boil into dry product NMP, water and low-boiling-point substance enter water return tank by tower top discharge through condensation and are circulated by pumped back atmospheric tower, dry product NMP is through vacuum suction rectifying tower, through condensation laggard NMP fine work tank after de-height boils.
Wherein, described copper-based catalysts is Cu-Zn/AL 2o 3.
In Wan Tong workshop section, GBL fine work and mass concentration be 40% Monomethylamine solution by volume 1:1.1 enter alkane reactive ketone bed after mixing.
In Wan Tong workshop section, methylamine decomposition tower ejects the methylamine gas come, in first absorber, pass through cyclic absorption, again the solution in first absorber is delivered to secondary absorber, and make the methylamine solution of 40% with single methylamine in secondary absorber, then for reaction.
In described lactone workshop section, the pressure of negative pressure tower is-0.072/-0.070MPa, and temperature is 170 DEG C/95 DEG C.
In described lactone workshop section, the pressure of rectifying tower is-0.089/-0.085 MPa, and temperature is 140 DEG C/120 DEG C.
In Wan Tong workshop section, the pressure of negative pressure tower is-0.065/-0.028MPa, and temperature is 165 DEG C/85 DEG C.
In Wan Tong workshop section, the pressure of rectifying tower is-0.089/-0.085 MPa, and temperature is 145 DEG C/120 DEG C.
The continuous production method of a kind of NMP, controlled by DCS, comprise lactone workshop section and Wan Tong workshop section, its detailed step is, described lactone workshop section: first with by preheat coil tail gas, preheating is carried out to butyleneglycol, be heated to 80-90 DEG C, hydrogen utilizes reactor gaseous phase materials to be out heated to 160-180 DEG C from normal temperature by hydrogen preheater, and gaseous phase materials utilizes reactor gaseous phase materials second-heating butyleneglycol out to 130 DEG C by butyleneglycol interchanger more afterwards; Then vaporizer is entered in the same way, hydrogen alcohol mol ratio 10:1-5:1, vaporization temperature: 190-210 DEG C, pressure: 0.06-0.09Mpa; Butyleneglycol enters superheater after vaporizing completely, through heat-conducting oil heating, and superheater temperature: 210-230 DEG C, pressure: 0.06-0.09Mpa; Enter reactor again at copper-based catalysts (Cu-Zn/AL 2o 3) there is lower reaction, the temperature 220-250 DEG C of reactor, pressure: 0.06-0.09Mpa; The butyrolactone generated and the gas mixture of hydrogen first pass through hydrogen interchanger, afterwards by after the heat exchange of butyleneglycol interchanger two step, 40-80 DEG C is cooled to after entering first step condenser and second stage condenser condenses again, enter GBL crude product tank, GBL crude product purity 97-99%; Surge tank before non-condensable gas air inlet fan, a part of hydrogen is emptying, and a part delivers to hydrogen recycle by blower fan; Butyrolactone in crude product tank is by being pumped to negative pressure tower, pressure is-0.072/-0.070MPa, temperature is 95-170 DEG C, carry out de-low boil and water obtain dry product GBL, dry product GBL is by vacuum suction rectifying tower, pressure is-0.089/-0.085, and temperature is 120 DEG C-140 DEG C, delivers to GBL fine work tank after de-height boils after condensation;
Described Wan Tong workshop section: GBL fine work and mass concentration be 40% Monomethylamine solution by volume 1:1.1 enter alkane reactive ketone bed after mixing, under high-temperature and high-pressure conditions, fully NMP crude product is produced in reaction, wherein temperature of reaction is 265-285 DEG C, reaction pressure is 6.5-8.0MPa, the purity of NMP crude product is 94-96%, the NMP crude product obtained enters atmospheric tower flash distillation again and anhydrates and point become with Monomethylamine semi-dried product to enter crude product tank, Monomethylamine and moisture are discharged after the laggard methylamine withdrawing can of condensation by being pumped to the process of methylamine decomposition tower by tower top, methylamine decomposition tower ejects the methylamine gas come, in first absorber, pass through cyclic absorption, again the solution in first absorber is delivered to secondary absorber, and the methylamine solution of 40% is made with single methylamine in secondary absorber, then for reaction, semi-dried product NMP is by being pumped to negative pressure tower, pressure is-0.065/-0.028MPa, temperature is 165 DEG C-85 DEG C, de-lowly boil into dry product NMP, water and low-boiling-point substance enter water return tank by tower top discharge through condensation and are circulated by pumped back atmospheric tower, and dry product NMP is through vacuum suction rectifying tower, and pressure is-0.089/-0.085 MPa, temperature is 145 DEG C/120 DEG C, through condensation laggard NMP fine work tank after de-height boils.
Described butyleneglycol (BDO) interchanger has gas, liquid separating apparatus; Described hydrogen preheater has vapour, liquid separating apparatus.
Described reactor is the reactor of two or more parallel connection, and the feed inlet end of each reactor is provided with control valve, when needing again to feed in raw material after producing, opens standby reactor, ensure that the continuity of production, improve production efficiency.
Reaction equation of the present invention is as follows:
Beneficial effect of the present invention is:
Technique of the present invention only has lactone and Wan Tongliangge workshop section, the pressure reduction of material qualified in negative pressure tower by existing between two towers, directly from negative pressure tower to rectifying tower punishment in advance, operation is energy-efficient, and whole technologist's proportioning is few, level of automation is high, unit consumption is low, good product quality, output are high.
40% methylamine solution of reaction, for recycling in technique the waste water that produces and Monomethylamine sterling is prepared voluntarily, and have the device reclaiming methylamine in waste water, advantage is the security that both ensure that production, turn avoid the process of the water of 60%, solved the excess amine of rectifying precipitation by recycling, the waste water of 180 kgs/tonne of NMP of generation is by sewage disposal qualified discharge.Make waste water generation in production process decrease 600 kgs/tonne of NMP, also effectively reduce production energy consumption, whole set process is environmental protection more economically.
Slave unit is said, eliminates the dry product tank in the middle of negative pressure tower to rectifying tower and some auxiliary facilitys thereof, adopt efficient advanced DCS operating system, reduce unit consumption, saved manpower and materials.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below by embodiment, technical scheme of the present invention is described in detail.
embodiment 1
Controlled by DCS, comprise lactone workshop section and Wan Tong workshop section, its detailed step is,
Described lactone workshop section: first with by preheat coil tail gas, preheating is carried out to butyleneglycol, be heated to 80 DEG C, hydrogen utilizes reactor gaseous phase materials to be out heated to 160 DEG C from normal temperature by hydrogen preheater, and gaseous phase materials utilizes reactor gaseous phase materials second-heating butyleneglycol out to 130 DEG C by butyleneglycol interchanger more afterwards; Then vaporizer is entered in the same way, hydrogen alcohol mol ratio 10:1, vaporization temperature: 190 DEG C, pressure: 0.06Mpa; Butyleneglycol enters superheater after vaporizing completely, through heat-conducting oil heating, and superheater temperature: 210 DEG C, pressure: 0.06Mpa; Enter reactor again at copper-based catalysts (Cu-Zn/AL 2o 3) there is lower reaction, the temperature of reactor 220 DEG C, pressure: 0.06Mpa; The butyrolactone generated and the gas mixture of hydrogen, first by hydrogen interchanger, afterwards by after the heat exchange of butyleneglycol interchanger two step, then be cooled to 40 DEG C after entering first step condenser and second stage condenser condenses, enter GBL crude product tank, GBL crude product purity 97%; Surge tank before non-condensable gas air inlet fan, a part of hydrogen is emptying, and a part delivers to hydrogen recycle by blower fan; Butyrolactone in crude product tank is by being pumped to negative pressure tower, and pressure is-0.072MPa, and temperature is 95 DEG C, carry out de-low boil and water obtain dry product GBL, dry product GBL is by vacuum suction rectifying tower, and pressure is-0.089 Mpa, temperature is 120 DEG C, delivers to GBL fine work tank after de-height boils after condensation;
Described Wan Tong workshop section: GBL fine work and mass concentration be 40% Monomethylamine solution by volume 1:1.1 enter alkane reactive ketone bed after mixing, under high-temperature and high-pressure conditions, fully NMP crude product is produced in reaction, wherein temperature of reaction is 265 DEG C, reaction pressure is 6.5MPa, the purity of NMP crude product is 94%, the NMP crude product obtained enters atmospheric tower flash distillation again and anhydrates and point become with Monomethylamine semi-dried product to enter crude product tank, Monomethylamine and moisture are discharged after the laggard methylamine withdrawing can of condensation by being pumped to the process of methylamine decomposition tower by tower top, methylamine decomposition tower ejects the methylamine gas come, in first absorber, pass through cyclic absorption, again the solution in first absorber is delivered to secondary absorber, and the methylamine solution of 40% is made with single methylamine in secondary absorber, then for reaction, semi-dried product NMP is by being pumped to negative pressure tower, pressure is-0.065MPa, temperature is 165 DEG C de-low and boils into dry product NMP, water and low-boiling-point substance enter water return tank by tower top discharge through condensation and are circulated by pumped back atmospheric tower, dry product NMP is through vacuum suction rectifying tower, pressure is-0.089 MPa, and temperature is 145 DEG C, through condensation laggard NMP fine work tank after de-height boils.
embodiment 2
Controlled by DCS, comprise lactone workshop section and Wan Tong workshop section, its detailed step is,
Described lactone workshop section: first with by preheat coil tail gas, preheating is carried out to butyleneglycol, be heated to 90 DEG C, hydrogen utilizes reactor gaseous phase materials to be out heated to 180 DEG C from normal temperature by hydrogen preheater, and gaseous phase materials utilizes reactor gaseous phase materials second-heating butyleneglycol out to 130 DEG C by butyleneglycol interchanger more afterwards; Then vaporizer is entered in the same way, hydrogen alcohol mol ratio 5:1, vaporization temperature: 210 DEG C, pressure: 0.09Mpa; Butyleneglycol enters superheater after vaporizing completely, through heat-conducting oil heating, and superheater temperature: 230 DEG C, pressure: 0.09Mpa; Enter reactor again at copper-based catalysts (Cu-Zn/AL 2o 3) there is lower reaction, the temperature of reactor 250 DEG C, pressure: 0.09Mpa; The butyrolactone generated and the gas mixture of hydrogen, first by hydrogen interchanger, afterwards by after the heat exchange of butyleneglycol interchanger two step, then be cooled to 80 DEG C after entering first step condenser and second stage condenser condenses, enter GBL crude product tank, GBL crude product purity 99%; Surge tank before non-condensable gas air inlet fan, a part of hydrogen is emptying, and a part delivers to hydrogen recycle by blower fan; Butyrolactone in crude product tank is by being pumped to negative pressure tower, and pressure is-0.070MPa, and temperature is 170 DEG C, carry out de-low boil and water obtain dry product GBL, dry product GBL is by vacuum suction rectifying tower, and pressure is-0.085, temperature is 140 DEG C, delivers to GBL fine work tank after de-height boils after condensation;
Described Wan Tong workshop section: GBL fine work and mass concentration be 40% Monomethylamine solution by volume 1:1.1 enter alkane reactive ketone bed after mixing, under high-temperature and high-pressure conditions, fully NMP crude product is produced in reaction, wherein temperature of reaction is 285 DEG C, reaction pressure is 8.0MPa, the purity of NMP crude product is 96%, the NMP crude product obtained enters atmospheric tower flash distillation again and anhydrates and point become with Monomethylamine semi-dried product to enter crude product tank, Monomethylamine and moisture are discharged after the laggard methylamine withdrawing can of condensation by being pumped to the process of methylamine decomposition tower by tower top, methylamine decomposition tower ejects the methylamine gas come, in first absorber, pass through cyclic absorption, again the solution in first absorber is delivered to secondary absorber, and the methylamine solution of 40% is made with single methylamine in secondary absorber, then for reaction, semi-dried product NMP is by being pumped to negative pressure tower, pressure is-0.028MPa, temperature is 85 DEG C, de-lowly boil into dry product NMP, water and low-boiling-point substance enter water return tank by tower top discharge through condensation and are circulated by pumped back atmospheric tower, and dry product NMP is through vacuum suction rectifying tower, and pressure is-0.085 MPa, temperature is 120 DEG C, through condensation laggard NMP fine work tank after de-height boils.

Claims (3)

1. the continuous production method of a NMP, the steps include: to be controlled by DCS, comprise lactone workshop section and Wan Tong workshop section, described lactone workshop section: first with by preheat coil tail gas, preheating is carried out to BDO, be heated to 80-90 DEG C, hydrogen utilizes reactor gaseous phase materials to be out heated to 160-180 DEG C from normal temperature by hydrogen preheater, gaseous phase materials utilizes reactor gaseous phase materials second-heating BDO out to 130 DEG C by BDO interchanger more afterwards; Then vaporizer is entered in the same way, hydrogen alcohol mol ratio 10:1-5:1, vaporization temperature: 190-210 DEG C, pressure: 0.06-0.09Mpa; BDO enters superheater after vaporizing completely, through heat-conducting oil heating, and superheater temperature: 210-230 DEG C, pressure: 0.06-0.09Mpa; Enter reactor reaction under copper-based catalysts exists again, described copper-based catalysts is Cu-Zn/AL 2o 3, the temperature 220-250 DEG C of reactor, pressure: 0.06-0.09Mpa; The butyrolactone generated and the gas mixture of hydrogen first pass through hydrogen interchanger, afterwards by 1, after the heat exchange of 4-butyleneglycol interchanger two step, be cooled to 40-80 DEG C after entering first step condenser and second stage condenser condenses again, enter GBL crude product tank, GBL crude product purity 97-99%; Surge tank before non-condensable gas air inlet fan, a part of hydrogen is emptying, and a part delivers to hydrogen recycle by blower fan; Butyrolactone in crude product tank is by being pumped to negative pressure tower, pressure is-0.072/-0.070MPa, temperature is 95-170 DEG C, carry out de-low boil and water obtain dry product GBL, dry product GBL is by vacuum suction rectifying tower, pressure is-0.089/-0.085 MPa, and temperature is 120 DEG C-140 DEG C, delivers to GBL fine work tank after de-height boils after condensation;
Described Wan Tong workshop section: GBL fine work and mass concentration be 40% Monomethylamine solution by volume 1:1.1 enter alkane reactive ketone bed after mixing, under high-temperature and high-pressure conditions, fully NMP crude product is produced in reaction, wherein temperature of reaction is 265-285 DEG C, reaction pressure is 6.5-8.0MPa, the purity of NMP crude product is 94-96%, the NMP crude product obtained enters atmospheric tower flash distillation again and anhydrates and point become with Monomethylamine semi-dried product to enter crude product tank, Monomethylamine and moisture are discharged after the laggard methylamine withdrawing can of condensation by being pumped to the process of methylamine decomposition tower by tower top, methylamine decomposition tower ejects the methylamine gas come, in first absorber, pass through cyclic absorption, again the solution in first absorber is delivered to secondary absorber, and the methylamine solution of 40% is made with single methylamine in secondary absorber, then for reaction, semi-dried product NMP is by being pumped to negative pressure tower, pressure is-0.065/-0.028MPa, temperature is 85 DEG C-165 DEG C, de-lowly boil into dry product NMP, water and low-boiling-point substance enter water return tank by tower top discharge through condensation and are circulated by pumped back atmospheric tower, and dry product NMP is through vacuum suction rectifying tower, and pressure is-0.089/-0.085 MPa, temperature is 120 DEG C-145 DEG C, through condensation laggard NMP fine work tank after de-height boils.
2. the continuous production method of NMP according to claim 1, is characterized in that, described BDO interchanger has gas, liquid separating apparatus; Described hydrogen preheater has vapour, liquid separating apparatus.
3. the continuous production method of NMP according to claim 1, it is characterized in that, described reactor is the reactor of two or more parallel connection, and the feed inlet end of each reactor is provided with control valve, when needing again to feed in raw material after producing, open standby reactor.
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CN106278983A (en) * 2015-06-05 2017-01-04 中国石化仪征化纤有限责任公司 A kind of N-Methyl pyrrolidone continuous preparation method
CN105085361A (en) * 2015-09-08 2015-11-25 江苏恒祥化工有限责任公司 System for synthesizing N-methyl-2-pyrrolidone
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