CN115181089B - Natural nicotine purifying process - Google Patents
Natural nicotine purifying process Download PDFInfo
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- CN115181089B CN115181089B CN202210697381.8A CN202210697381A CN115181089B CN 115181089 B CN115181089 B CN 115181089B CN 202210697381 A CN202210697381 A CN 202210697381A CN 115181089 B CN115181089 B CN 115181089B
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- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 79
- 229960002715 nicotine Drugs 0.000 title claims abstract description 79
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 68
- 230000008569 process Effects 0.000 title claims description 52
- 239000007788 liquid Substances 0.000 claims abstract description 138
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 238000000605 extraction Methods 0.000 claims abstract description 48
- 238000004821 distillation Methods 0.000 claims abstract description 47
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002351 wastewater Substances 0.000 claims abstract description 35
- 238000004062 sedimentation Methods 0.000 claims abstract description 34
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 238000010992 reflux Methods 0.000 claims abstract description 30
- 238000000746 purification Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 241000208125 Nicotiana Species 0.000 claims abstract description 20
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 17
- 239000000839 emulsion Substances 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 54
- 239000002904 solvent Substances 0.000 claims description 34
- 238000011084 recovery Methods 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000003921 oil Substances 0.000 claims description 17
- 230000001276 controlling effect Effects 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 239000010779 crude oil Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 238000004065 wastewater treatment Methods 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 6
- 239000008213 purified water Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 230000003113 alkalizing effect Effects 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims 4
- 230000008014 freezing Effects 0.000 claims 4
- 230000002950 deficient Effects 0.000 claims 2
- 239000002699 waste material Substances 0.000 abstract description 7
- YHBIGBYIUMCLJS-UHFFFAOYSA-N 5-fluoro-1,3-benzothiazol-2-amine Chemical compound FC1=CC=C2SC(N)=NC2=C1 YHBIGBYIUMCLJS-UHFFFAOYSA-N 0.000 description 7
- 238000005057 refrigeration Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000003571 electronic cigarette Substances 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/04—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond
Abstract
The invention designs a natural nicotine purification process, which is a production process for purifying tobacco extract raw materials with the nicotine content of 40 percent to more than or equal to 99.95 percent and the nicotine yield of more than or equal to 99.5 percent through the working procedures of anti-emulsifying agent preparation, alkalization treatment, extraction separation, standing sedimentation, wastewater separation, distillation desolventizing and rectification purification. The method specifically comprises the following steps: mixing raw materials, water and caustic soda according to a set proportion and a program to prepare an extract liquid, mixing the extract liquid with normal hexane to prepare an extract mixed liquid, standing and settling for 60 hours, discharging waste water after layering the extract mixed liquid, recovering clear liquid in the emulsion, and distilling and recycling normal hexane in the clear liquid, wherein the distilled raw materials are subjected to a high-proportion reflux rectification scheme comprises the following steps: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction, and recovering heavy clean oil to obtain high-purity nicotine product. Breaks through the limitations of low purity, low yield, large waste discharge and the like of the existing purification process, and has extremely high popularization value.
Description
Technical Field
The invention relates to a natural nicotine purification process, in particular to a production process for purifying a nicotine sulfate raw material with concentration of 40 percent to a purity of natural nicotine of more than 99.95 percent and a nicotine yield in the raw material of more than 99.5 percent by the process flow, belonging to the technical field of natural plant active ingredient purification process equipment.
Background
The nicotine is the effective component for cigarettes in the tobacco raw material, and the natural nicotine product is mainly used as a functional additive of an electronic cigarette atomized liquid, and is used for a small amount of medicines for stopping smoking and pesticides. The natural nicotine is obtained by processing a small amount of tobacco residue waste such as tobacco dust, crushed stems, tobacco fragments and the like which are generated in the tobacco processing process by a technology. The natural nicotine produced has small amounts of impurities, which are mainly flavour substances in tobacco. Due to the differences in various aspects such as tobacco producing areas, varieties, natural fermentation degrees and the like, the components of the impurities are different, and the differences in the fragrance and the aroma of the natural nicotine raw materials used in the electronic cigarette industry can be caused to a certain extent due to the impurity factors, namely, the purity of the natural nicotine raw materials is insufficient, and finally, the great differences (poor consistency) in the aroma of the electronic cigarette atomized liquid can be influenced, so that the product quality of the electronic cigarette is influenced.
The existing domestic and foreign known natural nicotine purification process comprises the following steps:
40% nicotine sulfate, alkalization treatment, extraction separation, distillation desolventizing, rectification purification and sealing storage
In the process, 40% of nicotine sulfate refers to: the liquid natural nicotine with the content of about 40 percent is obtained by alkalizing, extracting, distilling and rectifying the raw materials. Because the raw materials belong to valuables and have toxic and harmful risks to water ecology, the residues after extraction can be discharged after being treated, so that the improvement of purity and the increase of recovery yield are always important targets pursued in the industry.
The existing purification process has the defects that:
1. since the direct separation mode is adopted after extraction, the sufficient sedimentation separation time required for sedimentation separation of substances in the material is not given, so that the wastewater layer contains solvent and nicotine, and water-soluble impurities in the solvent cannot be effectively separated. The boiling point of nicotine is greatly reduced in the presence of water, so that the recovery rate of natural nicotine is insufficient, and the final comprehensive recovery rate is only about 83.5%.
2. In the rectification and purification process, a forced reflux pipe is not arranged, and although a small amount of rectification liquid naturally flows back in a rectification tower pipe in the rectification process, the ratio of the reflux quantity to the finished product collection quantity is too small (less than 10 percent), so that the removal of high-boiling-point impurities in materials is extremely unfavorable, and the final purity cannot reach an ideal target. Based on the above, the purity of the product purified by the process is generally only about 99.0% and the highest purity cannot be higher than 99.8% in the international and domestic industries at present.
3. In the process of production, the recovery rate of natural nicotine is an important index, and one of the disadvantageous factors of the insufficient recovery rate is that valuable raw materials are wasted, so that the purification cost is increased; and secondly, the pollution discharge pressure of the unrenewable raw materials which cannot be recycled is increased, so that the waste treatment cost is increased.
No introduction or publication is made on the aspects of checking the related technology in the aspect of purifying natural nicotine at home and abroad, wherein the comprehensive recovery rate is more than or equal to 99.5% and/or the product purity is more than or equal to 99.95%.
Disclosure of Invention
The invention aims at solving the problems in the background art, and designs a natural nicotine purification process, which is a production process for purifying a liquid 40% nicotine sulfate raw material, namely a tobacco extract with the nicotine content accounting for 40%, into a natural nicotine raw material with the purity of more than or equal to 99.95% and the nicotine yield of more than or equal to 99.5% through the process flow of the invention.
The technical scheme of the invention is as follows: a natural nicotine purification process is characterized in that:
the process comprises the following steps: preparing an anti-emulsifying agent, performing alkalization treatment, extracting and separating, standing and settling, separating waste water, distilling and desolventizing, and rectifying and purifying; the devices or equipment required in each process include: a material mixing tank 1, a material mixing tank 2, an extraction tank 3, a sedimentation tank 4, a pipeline filter 5, a clear liquid receiving tank 6, a pipeline sight glass 7, a No. 1 material conveying pump 8, a distillation column 9, a first condenser 10, a solvent recovery tank 11, a No. 2 material conveying pump 12, a solvent buffer tank 13, a feeding buffer tank 14, a rectifying column 15, a rectifying column pipe 16 with a stainless steel wire mesh filler arranged inside, a second condenser 17, a condensate buffer tank 18, an automatic forced reflux distributor 19, a qualified product receiving tank 20, a unqualified product receiving tank 21, a reflux pipe 22, a sample collecting valve 24 arranged in front of the reflux pipe 22 and a rectified liquid collecting pipe 25; also included are methods for detecting and controlling the operation of the respective devices or apparatus: the system comprises a vacuum pump, a negative pressure pipeline, a cooling water circulating pipeline, a chilled water circulating pipeline, a heat conducting oil circulating pipeline, a temperature sensor, a pressure sensor, a flowmeter, a liquid level meter, an electric control valve and a centralized control system; the 1# material conveying pump is used for conveying clear liquid, the 2# material conveying pump is used for conveying recyclable normal hexane, and the vacuum pump is used for pumping gas in a designated container and/or introducing materials required by negative pressure; the condensate buffer tank 18 receives the material flowing out of the condenser II 17 and flows to the automatic forced backflow distributor 19, a three-way valve for regulating the proportion of one inlet to two outlets is arranged in the automatic forced backflow distributor 19, one outlet is communicated with the upper part of the rectifying tower pipe 16 through a backflow pipe 22, and the other outlet is connected to the qualified product receiving tank 20 or the unqualified product receiving tank 21 through a rectifying liquid collecting pipe 25; the outside of the distillation tower 9 and the rectification tower 15 are respectively provided with a constant temperature heating jacket, and the inside of the first condenser 10 and the inside of the second condenser 17 are respectively provided with a heat exchange tube array;
the purification process comprises the following specific steps:
stp1, preparation of an anti-emulsifying agent: injecting a set amount of purified water into the batching tank 1 in a negative pressure mode, and slowly adding caustic soda with the set amount and purity more than or equal to 98% while stirring to prepare an anti-emulsifying agent; controlling the adding time of caustic soda to be more than or equal to 30min, stirring until the caustic soda is completely dissolved, and continuing stirring until the temperature of the anti-emulsifying agent in the material mixing tank 1 is reduced to 40-45 ℃;
stp2, alkalization treatment: the liquid 40% nicotine sulfate raw material to be purified is: the tobacco extract with the nicotine content of 40 percent is injected into the mixing tank 2 in a negative pressure sucking mode, and then the anti-emulsifying agent prepared according to stp1 is slowly added while stirring; controlling the adding time of the anti-emulsifying agent to be more than or equal to 30min, and continuously stirring for 90-120 min after the anti-emulsifying agent is completely added into the tobacco extract; preparing an extract;
stp3, extraction separation: firstly, injecting normal hexane with a set quantity into an extraction tank 3 in a negative pressure mode, and then adding an extraction liquid prepared according to stp2 while stirring; controlling the adding time of the extract to be more than or equal to 60min, and continuously stirring for 90-150min after the extract is completely added; completing the extraction process to obtain an extraction mixed solution;
stp4, standing and settling: delivering the extraction mixed liquor prepared according to stp3 into a settling tank 4 in a negative pressure mode; the extraction mixed liquor is free to settle in a standing state in the settling tank 4, and finally the material of the extraction mixed liquor is free to be layered due to density difference, wherein: the clear liquid with low density is positioned at the upper layer, the emulsified liquid with medium density is positioned at the middle layer, and the wastewater with high density is positioned at the lower layer; the clear liquid is an n-hexane solution extracted with nicotine components;
setting: the free sedimentation time of the extraction mixed liquor in a standing state is more than or equal to 60 hours;
stp5, wastewater separation: after stp4 reaches the setting time of standing and sedimentation, observing the liquid level and layering condition in the sedimentation tank 4, and discharging the wastewater through a valve arranged at the bottom of the sedimentation tank 4 until the liquid level of the wastewater in the sedimentation tank 4 is lower than the height of a clear liquid discharge port arranged on the sedimentation tank 4; respectively discharging clear liquid, waste water and emulsion by gravity flow, discharging the clear liquid into a clear liquid receiving tank 6, discharging the waste water into a waste water treatment temporary storage container, and discharging the emulsion for storage;
stp6, distilling to remove solvent; the clear liquid stored in the clear liquid receiving tank 6 is conveyed to the distillation tower 9 in batches through a No. 1 conveying pump, n-hexane in the clear liquid is separated through evaporation and condensation modes, the separated n-hexane is temporarily stored in the solvent recovery tank 11 while being distilled, and then conveyed to the solvent buffer tank 13 through a No. 2 conveying pump for extraction of raw materials in the next batch;
after the distillation desolventizing process is completed, the residual materials in the distillation tower are as follows: crude oil with the nicotine purity of more than or equal to 95 percent is conveyed to a feeding buffer tank 14 in a negative pressure conveying mode;
setting: the distillation temperature of the clear liquid in the distillation tower 9 is 80-140 ℃;
in the later stage of distillation, when the input flow of the solvent recovery tank 11 is measured to be less than 1% of the maximum flow, closing an evacuation valve arranged at the outlet of the solvent recovery tank 11, communicating the solvent recovery tank 11 with an external vacuumizing pipeline, and continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not drop and rise reversely, namely, the normal hexane in the clear liquid is completely distilled; then feeding nitrogen into the distillation tower to break the air, and closing the heating source;
stp7, rectification and purification: the rectification and purification comprises five links, namely: feeding and balancing temperature, front fraction collection, high-purity nicotine collection, rear fraction collection and recovery of heavy clean oil;
in the operation process, the adjustable effect of the flow ratio I value between the return pipe 22 and the rectifying liquid pipe 25 is realized by adjusting a proportion adjusting three-way valve arranged in the automatic forced return distributor 19;
the specific operation process of the method is as follows:
a. feed and equilibrium temperature: first, setting: the return pipe 22 is fully opened, the rectifying liquid collecting pipe 25 is closed, all the condensate flowing through the condensate buffer tank 18 flows back to the upper end of the rectifying tower pipe 16, namely the I value is infinite, and the vacuum degree in the rectifying tower 15 is higher than-0.09 Mpa; pumping the crude oil fed into the buffer tank 14 into the rectifying tower 15 and heating to 135+/-1 ℃, and setting the continuous evaporation and reflux time of the crude oil in the rectifying tower 15 in the constant temperature state to be as follows: 3-4 hours;
b. and (3) front fraction collection: extracting and analyzing a rectified liquid sample from the sample collecting valve 24 at fixed time, adjusting an I value= (5~3) when the content of single high-boiling-point impurities in the rectified liquid is less than or equal to 100mg/kg, and introducing the material flowing out of the rectified liquid pipe 25 into the reject receiving tank 21; when the purity of nicotine in the collected sample is more than or equal to 99.95%, the front distillation collection process is finished;
c. high purity nicotine fraction collection: keeping the I value as the set value in the step b, continuously rectifying, when the purity of nicotine in the collected sample is more than or equal to 99.95%, and the single high-boiling impurity content is more than 100mg/kg but less than 200mg/kg, immediately introducing the material flowing out of the rectifying liquid pipe 25 into the qualified product receiving tank 20 until the purity of nicotine in the sample is from high to low and is equal to 99.95%, stopping collecting fractions of high-purity nicotine, and closing a feeding valve communicated with the qualified product receiving tank 20 and the rectifying liquid pipe 25;
d. and (3) collecting a rear fraction: after step c is completed, the I value=0 is adjusted, i.e. the reflux is cut off, and the material flowing out of the rectification liquid pipe 25 is led into the reject receiving tank 21; d, rectifying tower 15 continues rectifying according to the temperature set in step a until the temperature in rectifying tower 15 is not increased and is not reversely reduced, and rectifying is finished; finally, the reject rectification liquid collected in the reject receiving tank 21 is refluxed to the clear liquid receiving tank 6;
e. recovering the heavy clean oil: after the rectification is finished, nitrogen is used for emptying and discharging the residual heavy clean oil in the rectification tower 15, and then the next rectification cycle process is carried out. Preferably, cooling jackets are arranged at the lower parts of the shells of the batching tank 1 and the mixing tank 2 and are used for accelerating the cooling of materials stored in the batching tank 1 and the mixing tank 2, and the cooling jackets are connected with cooling water circulation pipelines arranged outside; the first condenser 10 and the second condenser 17 are also respectively connected with cooling water circulation pipelines arranged outside; setting: the inlet temperature of the circulating cooling water is less than or equal to 30 ℃, and the return temperature is less than or equal to 35 ℃;
preferably, the lower parts of the shells of the acceptable product receiving tank 20 and the unacceptable product receiving tank 21 are provided with refrigeration jackets for storing the materials in the acceptable product receiving tank 20 and the unacceptable product receiving tank 21 under the low temperature condition, and the refrigeration jackets are connected with refrigeration water circulation pipelines arranged outside; setting: the inlet temperature of the circulating chilled water is less than or equal to 5 ℃, and the return temperature is less than or equal to 10 ℃;
further, in stp1, there is set: the weight ratio of the purified water to the caustic soda is 4: (0.8-1.2); in stp2, set is: the weight ratio of the anti-emulsifying agent to the tobacco extract with the nicotine content accounting for 40 percent is 5: (3.5 to 4.5); in stp3, set is: the weight ratio of the n-hexane to the extract is 13: (8-10);
further, fan-shaped propeller stirrers are arranged in the batching tank 1 and the mixing tank 2, and in the working process, the following steps are set: the rotating speed of the fan-shaped propeller stirrer is as follows: 90-120 rpm.
Preferably, three groups of stirrers which are coaxially distributed along the vertical direction are arranged in the extraction separation tank 3 and the distillation tower 9, and the three groups of stirrers are a fan-shaped propeller stirrer, a frame stirrer and a fan-shaped propeller stirrer from top to bottom in sequence, and the rotating speeds of the three groups of stirrers are as follows in the working process: 80-160 rpm.
Further, in the stp5, the discharged emulsion is further separated into the residual clear liquid in the emulsion by an oscillation demulsification method, and the separated clear liquid is led into a clear liquid receiving tank 6 and is discharged into a wastewater treatment temporary storage container to be led into a wastewater harmless treatment device.
Furthermore, in the stp7, a pipeline pump or a metering pump is connected in series between the automatic forced reflux distributor 19 and the reflux pipe 22, and the centralized control system precisely controls the reflux amount of the rectification liquid through the pipeline pump or the metering pump.
The invention has the advantages and beneficial effects that:
1. compared with the prior art, the technical scheme of the invention has the most outstanding innovation points that: the process of standing and settling is added, and the settling time is set to be more than 60 hours, so that the precipitation and separation of the extracted materials are facilitated, the comprehensive recovery rate of the natural nicotine in the raw materials is improved to be more than 99.5%, the application of the raw materials is facilitated, and the environmental protection pressure is reduced.
2. By adopting the technical scheme of the invention, the reflux quantity I is set as 5~3 in the rectification process, which is greatly higher than the existing process which only depends on a natural reflux mode, so that the purity of the finished nicotine can reach more than 99.95%, and the invention is very beneficial to adapting to the purity requirement of the final user on the product.
3. The technical scheme of the invention has the advantages of less required equipment, easy realization of automatic operation, low energy consumption of unit products, high comprehensive utilization rate of raw materials, less waste discharge and low cost for waste treatment.
4. The technical scheme of the invention has high popularization value.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a diagram showing an apparatus configuration according to an embodiment of the present invention;
FIG. 3 is an enlarged schematic view of the condensing and reflux apparatus of the rectifying and purifying section of FIG. 2;
FIG. 4 is a process flow diagram of a first embodiment of the present invention.
Description of the marks in the accompanying drawings:
in FIGS. 2 and 3, 1-batch tank, 2-mixing tank, 3-extraction tank, 4-settling tank, 5-pipeline filter, 6-clear liquid receiving tank, 7-pipeline mirror, 8-1 # feed pump, 9-distillation column, 10-condenser I, 11-solvent recovery tank, 12-2 # feed pump, 13-solvent buffer tank, 14-feed buffer tank, 15-rectifying column, 16-rectifying column pipe, 17-condenser II, 18-condensate buffer tank, 19-automatic forced reflux distributor, 20-acceptable product receiving tank, 21-unacceptable product receiving tank, 22-reflux pipe, 24-sample collecting valve, 25-rectifying liquid collecting pipe.
Detailed Description
Embodiments of the present invention are further described below with reference to the drawings, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below are exemplary and intended to illustrate the present invention and should not be construed as limiting the invention, but any modifications, equivalent substitutions or improvements made within the spirit and principles of the present invention should be included within the scope of the claims of the present invention, which are not described in detail in the present technical solution.
Referring to fig. 1 to 3, the process for purifying natural nicotine of the present invention comprises: preparing an anti-emulsifying agent, alkalizing, extracting and separating, standing and settling, separating waste water, distilling and desolventizing, and rectifying and purifying.
The devices or equipment required in each process include: a material mixing tank 1, a material mixing tank 2, an extraction tank 3, a sedimentation tank 4, a pipeline filter 5, a clear liquid receiving tank 6, a pipeline sight glass 7, a No. 1 material conveying pump 8, a distillation column 9, a first condenser 10, a solvent recovery tank 11, a No. 2 material conveying pump 12, a solvent buffer tank 13, a feeding buffer tank 14, a rectifying column 15, a rectifying column pipe 16 with a stainless steel wire mesh filler arranged inside, a second condenser 17, a condensate buffer tank 18, an automatic forced reflux distributor 19, a qualified product receiving tank 20, a unqualified product receiving tank 21, a reflux pipe 22, a sample collecting valve 24 arranged in front of the reflux pipe 22 and a rectified liquid collecting pipe 25; also included are methods for detecting and controlling the operation of the respective devices or apparatus: the system comprises a vacuum pump, a negative pressure pipeline, a cooling water circulating pipeline, a chilled water circulating pipeline, a heat conducting oil circulating pipeline, a temperature sensor, a pressure sensor, a flowmeter, a liquid level meter, an electric control valve and a centralized control system.
The 1# material conveying pump is used for conveying clear liquid, the 2# material conveying pump is used for conveying recyclable normal hexane, and the vacuum pump is used for pumping gas in a designated container and/or introducing materials required by negative pressure; the condensate buffer tank 18 receives the material flowing out of the condenser II 17 and flows to the automatic forced backflow distributor 19, a three-way valve for regulating the proportion of one inlet to two outlets is arranged in the automatic forced backflow distributor 19, one outlet is communicated with the upper part of the rectifying tower pipe 16 through a backflow pipe 22, and the other outlet is connected to the qualified product receiving tank 20 or the unqualified product receiving tank 21 through a rectifying liquid collecting pipe 25; the outside of distillation column 9 and rectifying column 15 all is provided with constant temperature heating jacket, the inside of condenser one 10 and condenser two 17 all is provided with the heat exchange tubulation.
The batching jar 1, compounding jar 2 are provided with fan-shaped screw agitator, set for in the work: the rotating speed of the fan-shaped propeller stirrer is as follows: 90-120 rpm; three groups of stirrers which are coaxially distributed along the vertical direction are arranged in the extraction separation tank 3 and the distillation tower 9, and the three groups of stirrers are a fan-shaped propeller stirrer, a frame stirrer and a fan-shaped propeller stirrer from top to bottom in sequence, and the rotating speeds of the three groups of stirrers are as follows in the working process: 80-160 rpm.
The lower parts of the shells of the batching tank 1 and the mixing tank 2 are provided with cooling jackets, the cooling jackets are used for accelerating the cooling of materials stored in the batching tank 1 and the mixing tank 2, and the cooling jackets are connected with cooling water circulation pipelines arranged outside; the first condenser 10 and the second condenser 17 are also respectively connected with cooling water circulation pipelines arranged outside; setting: the inlet temperature of the circulating cooling water is less than or equal to 30 ℃, and the return temperature is less than or equal to 35 ℃.
The lower parts of the shells of the acceptable product receiving tank 20 and the unacceptable product receiving tank 21 are provided with refrigeration jackets which are used for storing materials in the acceptable product receiving tank 20 and the unacceptable product receiving tank 21 under the low-temperature condition, and the refrigeration jackets are connected with refrigeration water circulation pipelines arranged outside; setting: the inlet temperature of the circulating chilled water is less than or equal to 5 ℃, and the return temperature is less than or equal to 10 ℃.
The purification process comprises the following specific steps:
stp1, preparation of an anti-emulsifying agent: injecting a set amount of purified water into the batching tank 1 in a negative pressure mode, and slowly adding caustic soda with the set amount and purity more than or equal to 98% while stirring to prepare an anti-emulsifying agent; controlling the adding time of caustic soda to be more than or equal to 30min, stirring until the caustic soda is completely dissolved, and continuing stirring until the temperature of the anti-emulsifying agent in the material mixing tank 1 is reduced to 40-45 ℃; setting: the weight ratio of the purified water to the caustic soda is 4: (0.8-1.2);
stp2, alkalization treatment: the liquid 40% nicotine sulfate raw material to be purified is: the tobacco extract with the nicotine content of 40 percent is injected into the mixing tank 2 in a negative pressure sucking mode, and then the anti-emulsifying agent prepared according to stp1 is slowly added while stirring; controlling the adding time of the anti-emulsifying agent to be more than or equal to 30min, and continuously stirring for 90-120 min after the anti-emulsifying agent is completely added into the tobacco extract; preparing an extract; setting: the weight ratio of the anti-emulsifying agent to the tobacco extract with the nicotine content accounting for 40 percent is 5: (3.5 to 4.5);
stp3, extraction separation: firstly, injecting normal hexane with a set quantity into an extraction tank 3 in a negative pressure mode, and then adding an extraction liquid prepared according to stp2 while stirring; controlling the adding time of the extract to be more than or equal to 60min, and continuously stirring for 90-150min after the extract is completely added; completing the extraction process to obtain an extraction mixed solution; setting: the weight ratio of the n-hexane to the extract is 13: (8-10);
stp4, standing and settling: delivering the extraction mixed liquor prepared according to stp3 into a settling tank 4 in a negative pressure mode; the extraction mixed liquor is free to settle in a standing state in the settling tank 4, and finally the material of the extraction mixed liquor is free to be layered due to density difference, wherein: the clear liquid with low density is positioned at the upper layer, the emulsified liquid with medium density is positioned at the middle layer, and the wastewater with high density is positioned at the lower layer; the clear liquid is an n-hexane solution extracted with nicotine components;
setting: the free sedimentation time of the extraction mixed liquor in a standing state is more than or equal to 60 hours;
stp5, wastewater separation: after stp4 reaches the setting time of standing and sedimentation, observing the liquid level and layering condition in the sedimentation tank 4, and discharging the wastewater through a valve arranged at the bottom of the sedimentation tank 4 until the liquid level of the wastewater in the sedimentation tank 4 is lower than the height of a clear liquid discharge port arranged on the sedimentation tank 4; respectively discharging clear liquid, waste water and emulsion by gravity flow; and discharging the clear liquid into a clear liquid receiving tank 6, discharging the wastewater into a wastewater treatment temporary storage container, further separating the clear liquid remained in the emulsion by an oscillation demulsification method after the emulsion is discharged, guiding the separated clear liquid into the clear liquid receiving tank 6, and guiding the wastewater discharged into the wastewater treatment temporary storage container into a wastewater harmless treatment device;
stp6, distilling to remove solvent; the clear liquid stored in the clear liquid receiving tank 6 is conveyed to the distillation tower 9 in batches through a No. 1 conveying pump, n-hexane in the clear liquid is separated through evaporation and condensation modes, the separated n-hexane is temporarily stored in the solvent recovery tank 11 while being distilled, and then conveyed to the solvent buffer tank 13 through a No. 2 conveying pump for extraction of raw materials in the next batch;
after the distillation desolventizing process is completed, the residual materials in the distillation tower are as follows: crude oil with the nicotine purity of more than or equal to 95 percent is conveyed to a feeding buffer tank 14 in a negative pressure conveying mode;
setting: the distillation temperature of the clear liquid in the distillation tower 9 is 80-140 ℃;
in the later stage of distillation, when the input flow of the solvent recovery tank 11 is measured to be less than 1% of the maximum flow, closing an evacuation valve arranged at the outlet of the solvent recovery tank 11, communicating the solvent recovery tank 11 with an external vacuumizing pipeline, and continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not drop and rise reversely, namely, the normal hexane in the clear liquid is completely distilled; then feeding nitrogen into the distillation tower to break the air, and closing the heating source;
stp7, rectification and purification: the rectification and purification comprises five links, namely: feeding and balancing temperature, front fraction collection, high-purity nicotine collection, rear fraction collection and recovery of heavy clean oil;
in the operation process, the adjustable effect of the flow ratio I value between the return pipe 22 and the rectifying liquid pipe 25 is realized by adjusting a proportion adjusting three-way valve arranged in the automatic forced return distributor 19;
the specific operation process of the method is as follows:
a. feed and equilibrium temperature: first, setting: the return pipe 22 is fully opened, the rectifying liquid collecting pipe 25 is closed, all the condensate flowing through the condensate buffer tank 18 flows back to the upper end of the rectifying tower pipe 16, namely the I value is infinite, and the vacuum degree in the rectifying tower 15 is higher than-0.09 Mpa; pumping the crude oil fed into the buffer tank 14 into the rectifying tower 15 and heating to 135+/-1 ℃, and setting the continuous evaporation and reflux time of the crude oil in the rectifying tower 15 in the constant temperature state to be as follows: 3-4 hours;
b. and (3) front fraction collection: extracting and analyzing a rectified liquid sample from the sample collecting valve 24 at fixed time, adjusting an I value= (5~3) when the content of single high-boiling-point impurities in the rectified liquid is less than or equal to 100mg/kg, and introducing the material flowing out of the rectified liquid pipe 25 into the reject receiving tank 21; when the purity of nicotine in the collected sample is more than or equal to 99.95%, the front distillation collection process is finished;
c. high purity nicotine fraction collection: keeping the I value as the set value in the step b, continuously rectifying, when the purity of nicotine in the collected sample is more than or equal to 99.95%, and the single high-boiling impurity content is more than 100mg/kg but less than 200mg/kg, immediately introducing the material flowing out of the rectifying liquid pipe 25 into the qualified product receiving tank 20 until the purity of nicotine in the sample is from high to low and is equal to 99.95%, stopping collecting fractions of high-purity nicotine, and closing a feeding valve communicated with the qualified product receiving tank 20 and the rectifying liquid pipe 25; d. and (3) collecting a rear fraction: after step c is completed, the I value=0 is adjusted, i.e. the reflux is cut off, and the material flowing out of the rectification liquid pipe 25 is led into the reject receiving tank 21; d, rectifying tower 15 continues rectifying according to the temperature set in step a until the temperature in rectifying tower 15 is not increased and is not reversely reduced, and rectifying is finished; finally, returning the unqualified rectifying liquid collected by the unqualified product receiving tank 21 to the clear liquid receiving tank 6;
e. recovering the heavy clean oil: after the rectification is finished, nitrogen is used for emptying and discharging the residual heavy clean oil in the rectification tower 15, and then the next rectification cycle process is carried out.
The technical scheme of the invention is further described by a specific embodiment
Embodiment one:
referring to fig. 4, 2 and 3, the raw material of the tobacco extract with the nicotine content of 40% required for single purification is 400kg, and other main raw materials required by the purification process of the invention are respectively as follows: 100kg of caustic soda with purity more than or equal to 98%, 400kg of tap water, 1300kg of normal hexane, a small amount of nitrogen, and cooling water and chilled water required by the production process are recycled, so that almost no loss is caused. Chilled water is prepared by a refrigerating unit, and the following steps are set: the temperature of the chilled water inlet and return water is respectively as follows: tap water is selected as cooling water at the temperature of 5 ℃ and 10 ℃, and the inlet and return temperatures of the cooling water are respectively set as follows: the heating source required in the distillation and rectification process at 20 ℃ and 30 ℃ is a heat conduction oil circulation pipeline, and the following steps are set: the heat conduction oil inlet and return temperatures are respectively as follows: 160℃and 155 ℃. The specific purification process comprises the following steps:
stp1, preparation of an anti-emulsifying agent: injecting tap water into the batching tank 1 in a negative pressure mode, and slowly adding caustic soda while stirring to prepare an anti-emulsifying agent; controlling the adding time of caustic soda for 35min, stirring until the caustic soda is completely dissolved, continuing stirring until the temperature of the anti-emulsifying agent in the preparation tank 1 is lower than 40 ℃ by matching with the cooling circulation effect of tap water outside the preparation tank; the stirring speed is 100 revolutions/min by adopting a fan-blade-shaped arc stirrer, wherein the diameter of the fan blade is 400 mm.
stp2, alkalization treatment: injecting the raw materials to be purified into a mixing tank 2 in a negative pressure sucking mode, and slowly adding an anti-emulsifying agent prepared according to stp1 while stirring; controlling the adding time of the anti-emulsifying agent to be 40min, and continuously stirring for 90min after the anti-emulsifying agent is completely added into the tobacco extract; making into extractive solution.
stp3, extraction separation: 1300kg of normal hexane is injected into the extraction tank 3 in a negative pressure mode, and then extraction liquid prepared according to stp2 is added while stirring; controlling the adding time of the extract for 60min, and continuously stirring for 90min after the extract is completely added; and (3) completing the extraction process to obtain an extraction mixed solution.
stp4, standing and settling: all the extraction mixed liquor prepared according to stp3 is conveyed into a settling tank 4 in a negative pressure mode; the extraction mixed liquor is free to subside for 60 hours in a static state in a settling tank 4, and finally the material of the extraction mixed liquor is free to delaminate due to density difference, wherein: the clear liquid with low density is positioned at the upper layer, the emulsified liquid with medium density is positioned at the middle layer, and the wastewater with high density is positioned at the lower layer by about 700 kg; the clear liquid refers to an n-hexane solution extracted with nicotine components.
stp5, wastewater separation: after the sedimentation process is finished, observing the liquid level and layering condition in the sedimentation tank 4 through a pipeline viewing mirror 7 arranged on the sedimentation tank 4, and discharging part of wastewater through a valve arranged at the bottom of the sedimentation tank 4 until the liquid level of the wastewater is lower than the height of a clear liquid discharge port arranged on the sedimentation tank 4; respectively discharging clear liquid, waste water and emulsion by gravity flow; and discharging the clear liquid into a clear liquid receiving tank 6, discharging the wastewater into a wastewater treatment temporary storage container, further separating the clear liquid remained in the emulsion by an oscillation demulsification method after the emulsion is discharged, guiding the separated clear liquid into the clear liquid receiving tank 6, and guiding the wastewater discharged into the wastewater treatment temporary storage container into a wastewater harmless treatment device.
Stp6, distilling to remove solvent; the clear liquid stored in the clear liquid receiving tank 6 is delivered to the distillation tower 9 in batches by a No. 1 delivery pump, and the clear liquid is separated by evaporation and condensationThe separated normal hexane is temporarily stored in the solvent recovery tank 11 while being distilled, and then is conveyed to the solvent buffer tank 13 through the No. 2 conveying pump for the extraction of the next batch of nicotine sulfate raw materials. Setting: the distillation temperature of the clear liquid in the distillation tower 9 is 100+/-1 ℃, and after the distillation and desolventizing process is completed, the purity of the nicotine remained in the distillation tower 9 is not less than95% crude oil, which is then conveyed to the feed buffer tank 14 in a negative pressure transfer.
In the later stage of distillation, when the input flow of the solvent recovery tank 11 is measured to be less than 1% of the maximum flow, closing an evacuation valve arranged at the outlet of the solvent recovery tank 11, communicating the solvent recovery tank 11 with an external vacuumizing pipeline, and continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not drop and rise reversely, namely, the normal hexane in the clear liquid is completely distilled; then, nitrogen is fed into the distillation column to break the air, and the heating source is turned off.
Stp7, rectification and purification: the rectification and purification comprises four links, namely: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction, and recovering heavy clean oil.
In the operation process, the adjustable effect of the flow ratio I value between the return pipe 22 and the rectifying liquid pipe 25 is realized by adjusting the proportion adjusting three-way valve arranged in the automatic forced return distributor 19.
The specific operation process of the method is as follows:
a. feed and equilibrium temperature: first, setting: the return pipe 22 is fully opened, the rectifying liquid collecting pipe 25 is closed, all the condensate flowing through the condensate buffer tank 18 flows back to the upper end of the rectifying tower pipe 16, namely the I value is infinite, and the vacuum degree in the rectifying tower 15 is higher than-0.09 Mpa; pumping the crude oil fed into the buffer tank 14 into the rectifying tower 15 and heating to 135+/-1 ℃, and setting the continuous evaporation and reflux time of the crude oil in the rectifying tower 15 in the constant temperature state to be as follows: 3-4 hours.
b. And (3) front fraction collection: extracting and analyzing a rectified liquid sample from the sample collecting valve 24 at regular time, adjusting the I value to be=5 when the content of single high-boiling-point impurities in the rectified liquid is less than or equal to 100mg/kg, and guiding the material flowing out of the rectified liquid pipe 25 into the reject receiving tank 21; when the purity of nicotine in the collected sample is more than or equal to 99.95%, the front distillation collection process is finished; this process takes about 3 to 5 hours.
c. High purity nicotine fraction collection: keeping the I value as the set value in the step b, continuously rectifying, when the purity of nicotine in the collected sample is more than or equal to 99.95%, and the single high-boiling impurity content is more than 100mg/kg but less than 200mg/kg, immediately introducing the material flowing out of the rectifying liquid pipe 25 into the qualified product receiving tank 20 until the purity of nicotine in the sample is from high to low and is equal to 99.95%, stopping collecting fractions of high-purity nicotine, and closing a feeding valve communicated with the qualified product receiving tank 20 and the rectifying liquid pipe 25; this process takes about 13 to 15 hours. d. And (3) collecting a rear fraction: after step c is completed, the I value=0 is adjusted, i.e. the return pipe 22 is closed, and the material flowing out of the rectification liquid pipe 25 is introduced into the reject receiving tank 21; d, rectifying tower 15 continues rectifying according to the temperature set in step a until the temperature in rectifying tower 15 is not increased and is not reversely reduced, and rectifying is finished; finally, returning the unqualified rectifying liquid collected by the unqualified product receiving tank 21 to the clear liquid receiving tank 6; this process takes about 30 to 50 minutes.
e. Recovering the heavy clean oil: after the rectification is finished, about 5kg of heavy clean oil remained in the rectification tower 15 is discharged by using nitrogen to break the air, and then the next rectification cycle process is carried out.
Compared with the prior art, one of the most outstanding innovation points of the technical scheme is that a standing sedimentation process is added, and the sedimentation time is set to be more than 60 hours, so that the sedimentation and separation of the extracted materials are facilitated, the comprehensive recovery rate of the natural nicotine in the raw materials is improved to be more than 99.5%, the raw materials are applied completely, and the environmental protection pressure is reduced; secondly, the reflux quantity I is set to be 5-2.5 in the rectification process, which is greatly higher than the existing technology which only depends on a natural reflux mode, so that the purity of the finally obtained nicotine finished product can reach more than 99.95%, and the method is very beneficial to adapting to the purity requirement of the final user on the product; the technical scheme of the invention has the advantages of less required equipment, easy realization of automatic operation, low energy consumption of unit products, high comprehensive utilization rate of raw materials, less waste discharge, low cost for waste treatment and high popularization value.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," "fixedly attached," and the like are to be construed broadly and may be, for example, fixedly attached, detachably attached, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
Claims (5)
1. A natural nicotine purification process is a production process for purifying tobacco extract raw materials with the nicotine content of 40 percent by the working procedures of preparing an anti-emulsifying agent, alkalizing, extracting and separating, standing and settling, separating waste water, distilling and desolventizing, rectifying and purifying until the nicotine content is more than or equal to 99.95 percent and the nicotine yield is more than or equal to 99.5 percent;
the devices or equipment required in each process include: the device comprises a material mixing tank, an extraction tank, a sedimentation tank, a pipeline filter, a clear liquid receiving tank, a pipeline sight glass, a No. 1 material conveying pump, a distillation column, a first condenser, a solvent recycling tank, a No. 2 material conveying pump, a solvent buffer tank, a feeding buffer tank, a rectifying column pipe with a stainless steel wire gauze filler arranged therein, a second condenser, a condensate buffer tank, an automatic forced reflux distributor, a qualified product receiving tank, a unqualified product receiving tank, a reflux pipe, a sample collecting valve and a rectifying liquid collecting pipe; also included are methods for detecting and controlling the operation of the respective devices or apparatus: the system comprises a vacuum pump, a negative pressure pipeline, a cooling water circulating pipeline, a chilled water circulating pipeline, a heat conducting oil circulating pipeline, a temperature sensor, a pressure sensor, a flowmeter, a liquid level meter, an electric control valve and a centralized control system; the method is characterized in that:
the production process comprises the following steps:
stp1, preparation of an anti-emulsifying agent: injecting a set amount of purified water into a batching tank in a negative pressure mode, and slowly adding caustic soda with the set amount and purity more than or equal to 98% while stirring to prepare an anti-emulsifying agent; controlling the adding time of caustic soda to be more than or equal to 30min, stirring until the caustic soda is completely dissolved, and continuing stirring until the temperature of the anti-emulsifying agent in the material mixing tank is reduced to 40-45 ℃;
stp2, alkalization treatment: injecting the raw materials to be purified into a mixing tank in a negative pressure suction mode, and slowly adding an anti-emulsifying agent prepared according to stp1 while stirring; controlling the adding time of the anti-emulsifying agent to be more than or equal to 30min, and continuously stirring for 90-120 min after the anti-emulsifying agent is completely added into the tobacco extract; preparing an extract;
stp3, extraction separation: firstly, injecting normal hexane with a set quantity into an extraction tank in a negative pressure mode, and then adding an extraction liquid prepared according to stp2 while stirring; controlling the adding time of the extract to be more than or equal to 60min, and continuously stirring for 90-150min after the extract is completely added; completing the extraction process to obtain an extraction mixed solution;
stp4, standing and settling: conveying the extraction mixed liquor prepared according to stp3 into a settling tank in a negative pressure mode; the extraction mixed liquor is subjected to free sedimentation in a standing state in a sedimentation tank, and layering phenomenon occurs in the extraction mixed liquor due to density difference, and clear liquid, emulsion and wastewater are sequentially formed from top to bottom; the clear liquid is an n-hexane solution extracted with nicotine components;
setting: the free sedimentation time of the extraction mixed liquor in a standing state is more than or equal to 60 hours;
stp5, wastewater separation: after stp4 reaches the setting time of standing and sedimentation, observing the liquid level and layering condition in the sedimentation tank, and discharging the wastewater through a valve arranged at the bottom of the sedimentation tank until the liquid level of the wastewater in the sedimentation tank is lower than the height of a clear liquid discharge port arranged on the sedimentation tank; respectively discharging clear liquid, waste water and emulsion by gravity flow, wherein the clear liquid is discharged into a clear liquid receiving tank, the waste water is discharged into a waste water treatment temporary storage container, and the emulsion is discharged for storage;
stp6, distilling to remove solvent; the clear liquid stored in the clear liquid receiving tank is conveyed to the distillation tower in batches through a No. 1 conveying pump, n-hexane in the clear liquid is separated in an evaporation and condensation mode, the separated n-hexane is temporarily stored in the solvent recovery tank while being distilled, and then the separated n-hexane is conveyed to the solvent buffer tank through a No. 2 conveying pump for extracting raw materials in the next batch;
after the distillation desolventizing process is completed, the residual materials in the distillation tower are as follows: crude oil with the nicotine purity of more than or equal to 95 percent is conveyed to a feeding buffer tank in a negative pressure conveying mode;
setting: the distillation temperature of the clear liquid in the distillation tower is 80-140 ℃;
in the later stage of distillation, when the input flow of the solvent recovery tank is measured to be less than 1% of the maximum flow, closing an exhaust valve arranged at the outlet of the solvent recovery tank, communicating the solvent recovery tank with an external vacuumizing pipeline, continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not drop and rise reversely, then feeding nitrogen into the distillation tower to break the air, and closing a heating source;
stp7, rectification and purification: the rectification and purification comprises five links, namely: feeding and balancing temperature, front fraction collection, high-purity nicotine collection, rear fraction collection and recovery of heavy clean oil;
in the rectification and purification process, the adjustable flow ratio I value between the reflux pipe and the rectification liquid pipe is realized by adjusting a proportion adjusting three-way valve arranged in the automatic forced reflux distributor;
the specific operation process of the method is as follows:
a. feed and equilibrium temperature: first, setting: the condensate flows through the condensate buffer tank to be totally refluxed to the upper end of the rectifying tower pipe, namely, the I value is infinite, and the vacuum degree in the rectifying tower is higher than-0.09 Mpa; pumping crude oil fed into a buffer tank into a rectifying tower, heating to 135+/-1 ℃, and setting the continuous evaporation and reflux time of the crude oil in the rectifying tower at the constant temperature for 3-4 hours;
b. and (3) front fraction collection: extracting and analyzing a rectifying liquid sample from the sample collecting valve at regular time, adjusting an I value= (5~3) when the content of single high-boiling-point impurities in the rectifying liquid is less than or equal to 100mg/kg, and introducing the material flowing out of the rectifying liquid pipe into a defective product receiving tank; when the purity of nicotine in the collected sample is more than or equal to 99.95%, the front distillation collection process is finished;
c. high purity nicotine fraction collection: keeping the I value as the set value in the step b, continuously rectifying, when the purity of nicotine in the collected sample is more than or equal to 99.95%, and the single high-boiling impurity content is more than 100mg/kg but less than 200mg/kg, immediately introducing the material flowing out of the rectifying liquid pipe 25 into the qualified product receiving tank 20 until the purity of nicotine in the sample is from high to low and is equal to 99.95%, stopping collecting fractions of high-purity nicotine, and closing a feeding valve communicated with the qualified product receiving tank 20 and the rectifying liquid pipe 25;
d. and (3) collecting a rear fraction: after the step c is completed, the I value=0 is regulated, namely, the reflux is cut off, and the material flowing out of the rectifying liquid pipe is led into a defective product receiving tank; d, continuously rectifying the rectifying tower according to the temperature set in the step a until the temperature in the rectifying tower is not increased and is reversely reduced, and ending the rectification; finally, returning the unqualified rectifying liquid collected by the unqualified product receiving tank to the clear liquid receiving tank;
e. recovering the heavy clean oil: after the rectification is finished, nitrogen is used for breaking the air, and the residual heavy clean oil in the rectification tower is discharged, and then the next rectification cycle process is carried out.
2. A process for purifying natural nicotine according to claim 1, characterized in that: the lower parts of the shells of the material mixing tank and the material mixing tank are provided with cooling jackets, the cooling jackets are used for accelerating the cooling of materials stored in the material mixing tank and the material mixing tank, and the cooling jackets are connected with cooling water circulation pipelines arranged outside; the first condenser and the second condenser are also respectively connected with a cooling water circulation pipeline arranged outside; setting: the inlet temperature of the circulating cooling water is less than or equal to 30 ℃, and the return temperature is less than or equal to 35 ℃.
3. A process for purifying natural nicotine according to claim 1, characterized in that: the lower parts of the shells of the acceptable product receiving tank and the unacceptable product receiving tank are provided with freezing jackets, the freezing jackets are used for storing materials in the acceptable product receiving tank and the unacceptable product receiving tank under the low-temperature condition, and the freezing jackets are connected with a freezing water circulation pipeline arranged outside; setting: the inlet temperature of the circulating chilled water is less than or equal to 5 ℃, and the return temperature is less than or equal to 10 ℃.
4. A process for purifying natural nicotine according to claim 1, characterized in that: in stp1, set is: the weight ratio of the purified water to the caustic soda is 4: (0.8-1.2); in stp2, set is: the weight ratio of the anti-emulsifying agent to the tobacco extract with the nicotine content accounting for 40 percent is 5: (3.5 to 4.5); in stp3, set is: the weight ratio of the n-hexane to the extract is 13: (8-10).
5. A process for purifying natural nicotine according to claim 1, characterized in that: in stp5, the discharged emulsion is further separated to obtain the residual clear liquid in the emulsion by an oscillation demulsification method, and the separated clear liquid is introduced into a clear liquid receiving tank.
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| CN217988430U (en) * | 2022-06-20 | 2022-12-09 | 托拔克生物科技(衡阳)有限公司 | Natural nicotine purification system |
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| CN104428421A (en) * | 2012-07-13 | 2015-03-18 | 亲切消费者有限公司 | Process for using tobacco |
| CN105566288A (en) * | 2014-10-14 | 2016-05-11 | 北京本草通汇科技中心 | High purity nicotine industrial preparation method |
| CN112384504A (en) * | 2018-06-15 | 2021-02-19 | R.J.雷诺兹烟草公司 | Purification of nicotine |
| CN114605382A (en) * | 2020-12-04 | 2022-06-10 | 上海烟草集团有限责任公司 | Nicotine and preparation method thereof |
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