CN1106892C - Process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer - Google Patents
Process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer Download PDFInfo
- Publication number
- CN1106892C CN1106892C CN00116184A CN00116184A CN1106892C CN 1106892 C CN1106892 C CN 1106892C CN 00116184 A CN00116184 A CN 00116184A CN 00116184 A CN00116184 A CN 00116184A CN 1106892 C CN1106892 C CN 1106892C
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- Prior art keywords
- nicotine
- melanoid
- solvent
- composite fertilizer
- prepare
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Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
Abstract
The present invention provides a process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer. The raw material is put once to be used sufficiently. The present invention has perfect technology matching and simple flow, the present invention can extract and prepare more products in a selective way, and the extraction purity and the yield rate are improved essentially. The whole technology system digests cured tobacco material, the present invention brings no pollution, and the comprehensive production cost is reduced. The product has high quality, high oil purity, no impure gas and obvious fragrance increasing effect. The cured tobacco melanoid is transformed thoroughly, cigarette smoke gas is fragrant, and older cigarette fragrance is added. The purity of the nicotine is high, the purity is about more than 95%, and the nicotine can be used for a medicinal industry directly. The present invention has high yield which is 12 times as high as the traditional method. The present invention is a dual environmental protection type production technology which can reduce the production cost and improve the comprehensive economic benefit.
Description
The invention belongs to tobacco comprehensive utilization field, relate to and utilize the discarded tobacco material that produces in the cigarette process process, the method for the essence that the selective extraction added value is higher, spices and medicine industry raw material.More specifically to a kind of complementary recombining process from discarded tobacco material, selective extraction tobacco cleaned oil, melanoid, nicotine and prepare the method for composite fertilizer.
In the technological process of producing cigarette, can produce a large amount of discarded tobacco materials.These tobacco materials bring great hidden danger not only for environmental protection and fire-fighting, are again the cigarette low-grade raw material sources of faking, and not being used simultaneously also is a kind of huge waste.Be rich in a large amount of medical raw materials technologies such as extractible essence, spices and nicotine in fact in the tobacco, not only utility value height, and added value height, supply falls short of demand on market for its byproduct.Existing technology all is the single technology that is provided with at a certain extract basically, as the technology of extracting tobacco cleaned oil, the technology of extraction tobacco essential oil, technology of extraction tobacco extract or the like.These production technique not only selectivity are not high, and technology is coarse, and by product is many in the extract, and the finished product purity is low, and productive rate is not high.Some takes rectification process to the equipment requirements height.The inventor through concentrating on studies, has developed a kind of complementary compound novel process easy, that extract tobacco cleaned oil, melanoid, nicotine and prepare compoiste fertilizer efficiently at the shortcoming and defect of prior art.Through evidence, technology is easy, and extract purity height, productive rate also greatly improve.
The object of the present invention is to provide a kind of is raw material with the tankage tobacco in the cured tobacco production process, adopts the novel method of its tobacco cleaned oil that is rich in of complementary recombining process selective extraction, melanoid, nicotine and preparation compoiste fertilizer.Technical process of the present invention is as follows:
Concrete operation is as follows successively:
The flue-cured tobacco material is ground into the following fragment of 4mm, adds 5-9 doubly to the polar solvent of raw material, in 70-95 ℃ temperature range, and with 6-10r/min stirring and leaching 2-4 hour at a slow speed.Then, technology is filtered or press filtration routinely, separates flue-cured tobacco and organizes solid substance (filter residue) and leach liquor.
Filter residue is controlled in the scope of 13-15% the water ratio of material 95-110 ℃ of oven dry down.Under air-tight state, add 3-8 fat-soluble solvent doubly and soaked 12-24 hour.Technology is filtered routinely under air-tight state, and gravity leaches slag charge.Filtrate is at 95 ℃ of solvent flashings, and the normal temperature water-cooled is collected solvent, and enriched material is absolute oil.
Leach liquor after the polar solvent lixiviate, the ratio adding basifier in 0.1-5 ‰ fully stirs, and makes to react completely.Concentrate under 95-105 ℃ of temperature then, filtrate is condensed into the 1/5-1/10 of stoste volume, evaporable gas feeds in the water and collects thick nicotinic therebetween.With the technology layering extraction routinely of alkyl chloride kind solvent, 80-95 ℃ of volatilization normal temperature water-cooled collected solvent, concentrated and purified nicotine, and the brown bottle packing is preserved.
Solution is after concentrating after the alkalinisation treatment, and the product that heat filtering is got rid of behind the solid substance is melanoid.
After slag charge that produces in above-mentioned each operation and solid substance are collected, further solvent flashing under normal pressure, food sterilizing technology is carried out sterilising treatment routinely then.By the requirement of production different fertilizer, add the fertilizer nutrition-fortifying agent, make compoiste fertilizer.
In whole extraction process, material increases by one polar solvent lixiviate operation before traditional fat-soluble solvent lixiviate.Its purpose is the soluble composition wash-out of polar solvent is separated, and helps the separation of raising of final product absolute oil purity and melanoid.Conventional processes does not have polarity dissolving lixiviate, then all enters solution when the fat-soluble solvent lixiviate, has caused the reduction of absolute oil purity.
Polar solvent of the present invention is the methyl alcohol of 50% concentration, and formaldehyde and soft water can be finished the present invention.
The raw material that slag charge after a lixiviate, filtration extracts as absolute oil, its drying is extremely important, and it is comparatively suitable generally water content to be controlled between the 12-15%.The too high lixiviate that is unfavorable for fat-soluble solvent of water content may cause the reduction of absolute oil productive rate, purity.Cross the low luxus consumption that also can cause solvent in the next process, product cost raises.
The sherwood oil of boiling range during ethers, alcohols, alkane solvents generally can adopt, the alcohols of carbon below 5 is as ethanol, propyl alcohol etc.; The alkane solvents of carbon 4-6 is as normal hexane etc.
Solution after the polar solvent lixiviate is through alkalinisation treatment, basifier is generally highly basic such as HaOH, KOH, the highly basic of other types also can be realized purpose of the present invention, but should notice that basifier should not contain divalent-metal ion, otherwise easily produce precipitation in the operation afterwards, influence the isolation and purification of final product.
Conversion procedure is extremely important, and its purpose is through non-enzyme browning reaction polar component thoroughly to be converted into the melanoid of one of tobacco ageing product.
Thick nicotinic concentrates and purifies after extracting with the alkyl chloride kind solvent.General (technical grade) chloroform that adopts can be realized purpose of the present invention.Also can adopt methylene dichloride, ethylene dichloride etc. as extraction agent.
The present invention's technology both can prepare the tobacco planting compoiste fertilizer, also can prepare the compoiste fertilizer that other proportion of crop plantings use, and was the best with the former especially.
Complementary recombining process of the present invention has been realized the once input of raw material, full price utilization.Not only technical process is simplified, fecund product selective extraction and preparation, and the purity of extract, product have obtained substantial raising.Whole technology no longer produces any waste material, and the comprehensive cost of production reduces, and is a kind of double environmental protection type production technology.
The present invention is further illustrated below in conjunction with embodiment:
Embodiment one
Flue-cured tobacco material 100kg is ground into the following fragment of 4mm, adds 9 times to the polar solvent soft water of raw material (900kg), at 70-95 ℃ temperature range meat, and whisks lixiviate at a slow speed 3 hours with 6-10r/min.Then, technology is filtered routinely, separates flue-cured tobacco and organizes solid substance and leach liquor.
Filter residue is controlled in the scope of 13-15% the water ratio of material 95-110 ℃ of oven dry down.Under air-tight state, the middle boiling range sherwood oil that adds 8 times soaked 12 hours.Technology is filtered routinely under air-tight state, and gravity leaches slag charge.Filtrate is at 95 ℃ of solvent flashings, and the normal temperature water-cooled is collected solvent, and enriched material is absolute oil.Purity can reach 95%, and productive rate can reach 1.2%, output 1.2kg.
Leach liquor after the polar solvent lixiviate, the ratio in 0.1% add basifier solid NaOH, fully stir, and make to react completely.Concentrate under 95-105 ℃ of temperature then, filtrate is condensed into 1/5 of stoste volume, evaporable gas feeds in the soft water and collects thick nicotinic therebetween.With chloroform technology layering extraction routinely, solvent is reclaimed in the cooling of 80-95 ℃ of volatilization normal-temperature water, concentrated and purified nicotine, and the brown bottle packing is preserved.Nicotine productive rate 0.6%, i.e. 0.6kg.
Solution is after concentrating after the alkalinisation treatment, and the product that heat filtering is got rid of solid substance is melanoid, productive rate 2.6kg, i.e. 2.6kg.
After slag charge that produces in above-mentioned each operation and solid substance are collected, further solvent flashing under normal pressure, food sterilizing technology is carried out sterilising treatment routinely then.By the requirement of production different fertilizer, add the fertilizer nutrition-fortifying agent.As produce the flue-cured tobacco compoiste fertilizer, add each nitrogen phosphorus potassium additive of 15% in 1: 1: 1 ratio.The process heat extrusion molding is granulated routinely again, and is air-dry, makes compoiste fertilizer.Its productive rate is more than 200%, promptly more than the 200kg.
Embodiment two
Flue-cured tobacco material 100kg is ground into the fragment of 1mm, adds 7 times of formaldehyde to polar solvent 50% concentration of raw material (700kg), in 70-95 ℃ temperature range, and with 6-10r/min stirring and leaching 4 hours at a slow speed.Then, under the pressure about 1MPa, filter, separate flue-cured tobacco and organize solid substance and leach liquor.
Filter residue is dried under 95-110 ℃ of temperature, and the water ratio of material is controlled in the scope of 13-15%.Under air-tight state, the pentane that adds 3 times soaked 24 hours.Technology is filtered routinely under air-tight state, and gravity leaches slag charge.Filtrate is at 95 ℃ of solvent flashings, and the normal temperature water-cooled is collected solvent, and enriched material is absolute oil.Purity can reach 90%, and productive rate can reach 1.3%.
Leach liquor after the polar solvent lixiviate, the ratio in 5 ‰ add basifier solid NaOH, fully stir, and make to react completely.Concentrate under 95-105 ℃ of temperature then, filtrate is condensed into 1/10 of stoste volume, evaporable gas feeds in the soft water and collects thick nicotinic therebetween.With ethylene dichloride technology layering extraction routinely, 80-95 ℃ of volatilization, normal temperature cooling down reclaims solvent, concentrated and purified nicotine, and the brown bottle packing is preserved.Make nicotine, its productive rate 0.6%, i.e. 0.6kg.Can replace NaOH with KOH during alkalinisation treatment, its effect is suitable.
After the alkalinisation treatment solution through be concentrated into original volume 1/10 after, handle by the mode identical with embodiment one, make melanoid, its productive rate 2.6%, i.e. 2.6kg.
After the slag charge that produces in above-mentioned each operation and solid substance are collected, handle, make compoiste fertilizer, its productive rate 200%, i.e. 200kg by the mode identical with embodiment one.
Embodiment three
Flue-cured tobacco material 100kg is ground into the fragment of 0.5mm, adds 7 times of methyl alcohol to polar solvent 50% concentration of raw material (700kg), in 70-95 ℃ temperature range, and with 6-10r/min stirring and leaching 4 hours at a slow speed.Then, under the pressure about 0.5MPa, filter, separate flue-cured tobacco and organize solid substance and leach liquor.
Filter residue is dried under 95-110 ℃ of temperature, and the water ratio of material is controlled in the scope of 13-15%.Under air-tight state, add 5 times alcohol immersion 18 hours.Technology is filtered routinely under air-tight state, and gravity leaches slag charge.Filtrate is at 95 ℃ of solvent flashings, and the normal temperature water-cooled is collected solvent, and enriched material is absolute oil.Purity can reach 90%, and productive rate can reach 1.5%.
Leach liquor after the polar solvent lixiviate, the ratio in 0.75 ‰ add basifier solid NaOH, fully stir, and make to react completely.Concentrate under 95-105 ℃ of temperature then, filtrate is condensed into 1/8 of stoste volume, evaporable gas feeds in the soft water and collects thick nicotinic therebetween.With chloroform technology layering extraction routinely, 80-95 ℃ of volatilization, normal temperature cooling down reclaims solvent, concentrated and purified nicotine, and the brown bottle packing is preserved.Make nicotine, its productive rate is suitable with second embodiment.Can replace NaOH with KOH during alkalinisation treatment, its effect is suitable.
Solution is suitable with second embodiment through concentrating after the alkalinisation treatment.To original volume 1/8 after, handle by the mode identical with embodiment one, make melanoid, its productive rate is suitable with second embodiment.
After the slag charge that produces in above-mentioned each operation and solid substance are collected, handle by the mode identical with embodiment one, make compoiste fertilizer, its productive rate is suitable with second embodiment.
Embodiment four
Flue-cured tobacco material 100kg is ground into the fragment of 1mm, adds 8 times to the polarity soft water of raw material (800kg), in 70-95 ℃ temperature range, and with 6-10r/min stirring and leaching 4 hours at a slow speed.Then, under the pressure about 0.6MPa, filter, separate flue-cured tobacco and organize solid substance and leach liquor.
Filter residue is dried under 95-110 ℃ of temperature, and the water ratio of material is controlled in the scope of 13-15%.Under air-tight state, the normal hexane that adds 5 times soaked 14 hours.Technology is filtered routinely under air-tight state, and gravity leaches slag charge.Filtrate is at 95 ℃ of solvent flashings, and the normal temperature water-cooled is collected solvent, and enriched material is absolute oil.Purity can reach 95%, and productive rate can reach 1.3%.
Leach liquor after the polar solvent lixiviate, the ratio in 0.25 ‰ add basifier solid NaOH, fully stir, and make to react completely.Concentrate under 95-105 ℃ of temperature then, filtrate is condensed into 1/8 of stoste volume, evaporable gas feeds in the soft water and collects thick nicotinic therebetween.With methylene dichloride technology layering extraction routinely, 80-95 ℃ of volatilization, normal temperature cooling down reclaims solvent, concentrated and purified nicotine, and the brown bottle packing is preserved.Make nicotine, its productive rate is suitable with second embodiment.Can replace NaOH with KOH during alkalinisation treatment, its effect is suitable.
Solution is suitable with second embodiment through concentrating after the alkalinisation treatment.To original volume 1/8 after, handle by the mode identical with embodiment one, make melanoid, its productive rate is suitable with second embodiment.
After the slag charge that produces in above-mentioned each operation and solid substance are collected, handle by the mode identical with embodiment one, make compoiste fertilizer, its productive rate is suitable with second embodiment.
Characteristics of the present invention:,
1, process characteristic: (1) process matching, operation is complete, complementary combination process system digestion flue-cured tobacco Material, pollution-free; (2) substep selective extraction effective ingredient is conducive to the separation of intermediate product, The purifying of final products; (3) bad polarity composition thoroughly is converted into the tobacco ageing product in the flue-cured tobacco, Its value is able to Effective Raise; (4) productive rate height is high more than 12 times than conventional method; (5) not only Low for equipment requirements, and a cover explained hereafter four kinds of products nearly, system reduces production costs, Improve overall economic efficiency.
2, products characteristics: (1) flue-cured tobacco absolute oil purity height, there is not bad assorted gas, the flavouring effect is remarkable, can Strong with property; (2) the flue-cured tobacco melanoid transforms thoroughly, can make cigarette smoke pure and mild, increases Chen Yanxiang, makes High with being worth; (3) nicotine purity height generally more than 95%, can be directly used in medical industry. (4) The composite fertilizer of making can be directly used in the plantation of crops, particularly flue-cured tobacco.
Claims (8)
1, a kind ofly extract tobacco cleaned oil, melanoid, nicotine and prepare the method for composite fertilizer, the concrete operation of its recombining process flow process is as follows successively:
A, flue-cured tobacco material are ground into the following fragment of 4mm, add 5-9 doubly to the polar solvent of raw material, in 70-95 ℃ temperature range, and with 6-10r/min stirring and leaching 2-4 hour then at a slow speed, technology is filtered or press filtration routinely, separates flue-cured tobacco and organizes solid substance (filter residue) and leach liquor;
B, filter residue are controlled in the scope of 13-15% the water ratio of material 95-110 ℃ of oven dry down, under air-tight state, add in doubly ethers of 3-8, alcohols, the alkanes solvent soaking 12-24 hour.Technology is filtered routinely under air-tight state, and gravity leaches slag charge; Filtrate is at 95 ℃ of solvent flashings, and the normal temperature water-cooled is collected solvent, and enriched material is absolute oil;
Leach liquor after C, the polar solvent lixiviate, the ratio adding basifier in 0.1-5 ‰ fully stirs, make and react completely, concentrate under 95-105 ℃ of temperature then, filtrate is condensed into the 1/5-1/10 of stoste volume, evaporable gas feeds in the water and collects thick nicotinic therebetween; With the technology layering extraction routinely of alkyl chloride kind solvent, 80-95 ℃ of volatilization normal temperature water-cooled collected solvent, concentrated and purified nicotine, and the brown bottle packing is preserved;
Solution is after concentrating after D, the alkalinisation treatment, and the product that heat filtering is got rid of solid substance is melanoid;
After slag charge that produces in E, above-mentioned each operation and solid substance are collected, further solvent flashing under normal pressure, food sterilizing technology is carried out sterilising treatment routinely then, by the requirement of production different fertilizer, adds the fertilizer nutrition-fortifying agent, makes compoiste fertilizer.
2, extraction tobacco cleaned oil as claimed in claim 1, melanoid, nicotine and prepare the method for composite fertilizer is characterized in that: the amount of polar solvent be the material total amount 6-8 doubly; The time of stirring and leaching is 2-2.5 hour.
3, extraction tobacco cleaned oil as claimed in claim 1 or 2, melanoid, nicotine and prepare the method for composite fertilizer, it is characterized in that: the concentration of described polar solvent is 50%.
4, extraction tobacco cleaned oil as claimed in claim 1, melanoid, nicotine and prepare the method for composite fertilizer is characterized in that: the water ratio of dry back material is 13-14%; The amount of ethers, alcohols, alkane solvents is 4-6 a times of dry back slag charge amount; Extraction time is 14-18 hour.
5, as claim 1 or 4 described extraction tobacco cleaned oils, melanoid, nicotine and prepare the method for composite fertilizer, it is characterized in that: described ethers, alcohols, alkane solvents are middle boiling range sherwood oil, the carbon alcohols below 5, the alkane solvents of carbon 4-6.
6, as claim 1 or 4 described extraction tobacco cleaned oils, melanoid, nicotine and prepare the method for composite fertilizer, it is characterized in that: described basifier is solid NaOH, KOH, and its add-on is the 0.25-0.75 ‰ of amount of filtrate.
7, as claim 1 or 4 described extraction tobacco cleaned oils, melanoid, nicotine and prepare the method for composite fertilizer, it is characterized in that: the nicotine used chloroparaffin kind solvent of purifying is chloroform, methylene dichloride, ethylene dichloride.
8, as claim 1 or 4 described extraction tobacco cleaned oils, melanoid, nicotine and prepare the method for composite fertilizer, it is characterized in that: the pressure of described press filtration is 0.5-1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00116184A CN1106892C (en) | 2000-10-16 | 2000-10-16 | Process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00116184A CN1106892C (en) | 2000-10-16 | 2000-10-16 | Process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1296864A CN1296864A (en) | 2001-05-30 |
| CN1106892C true CN1106892C (en) | 2003-04-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00116184A Expired - Fee Related CN1106892C (en) | 2000-10-16 | 2000-10-16 | Process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer |
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| CN (1) | CN1106892C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103720029A (en) * | 2013-12-13 | 2014-04-16 | 云南中烟昆船瑞升科技有限公司 | Papermaking reconstituted tobacco extracting solution combination pre-treatment process |
| CN103689459B (en) * | 2013-12-13 | 2015-05-20 | 东北农业大学 | Method for preparing melanoidin with antioxidant activity |
| CN106396795A (en) * | 2016-08-29 | 2017-02-15 | 潘爱华 | Medium and trace element-containing organic water-soluble fertilizer produced from tobacco wastes |
| CN106278751A (en) * | 2016-08-29 | 2017-01-04 | 潘爱华 | A kind of organic water-soluble fertilizer utilizing tobacco leftovers to produce |
| CN110646372A (en) * | 2019-10-16 | 2020-01-03 | 江南大学 | Quantitative detection method of melanoidin |
| CN113475739B (en) * | 2021-07-10 | 2022-11-11 | 深圳市真味生物科技有限公司 | Preparation method of S-nicotine |
| CN114534361A (en) * | 2021-12-31 | 2022-05-27 | 南阳理工学院 | Method for combined extraction of essential oil, nicotine and extract from waste and inferior tobacco leaves |
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2000
- 2000-10-16 CN CN00116184A patent/CN1106892C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1296864A (en) | 2001-05-30 |
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