CN103483376B - Tobacco waste extracts the extraction process of inositol hexaphosphate calcium magnesium coproduction nicotine - Google Patents
Tobacco waste extracts the extraction process of inositol hexaphosphate calcium magnesium coproduction nicotine Download PDFInfo
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- CN103483376B CN103483376B CN201310437306.9A CN201310437306A CN103483376B CN 103483376 B CN103483376 B CN 103483376B CN 201310437306 A CN201310437306 A CN 201310437306A CN 103483376 B CN103483376 B CN 103483376B
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Abstract
The invention discloses the extracting method that a kind of tobacco waste extracts inositol hexaphosphate calcium magnesium coproduction nicotine, the method gets cigarette root, leaf, stalk or fireworks, pulverize, under slightly acidic condition, nicotine can first be extracted, and under this condition, phytic acid can not dissociate out, continue to adjust pH to be 2.0 ~ 3.0, phytic acid can be extracted, generate further inositol hexaphosphate calcium magnesium, the maximum advantage of this technique is by continuous setup pH value, synchronous production inositol hexaphosphate calcium magnesium and nicotine, reduce production cost; This technique extraction efficiency is high, can synchronously obtain Phytin and nicotine, greatly reduce the discharge of sewage, reduces production cost, has comparatively actual meaning for making full use of tobacco waste resource.
Description
Technical field
The present invention relates to the extraction process that a kind of tobacco waste extracts inositol hexaphosphate calcium magnesium coproduction nicotine.
Background technology
China's tobacco planting area is very large, has some amount tobacco leaf not to be used for production of cigarettes, leave a lot of stem stalk, root and fireworks the like waste simultaneously in recovery process, use can not, hesitate to discard.Containing number of chemical composition in tobacco waste, mainly comprise the materials such as alkaloid, protein, amino acid, glycoside, carbohydrate, organic acid.Wherein nicotine, Salanesol, organic acid, tobacco protein etc. all have higher utility value.To the comprehensive utilization of waste tobacco leaf, be subject to the attention of domestic and international investigator always, create a lot of comparatively ripe extraction process and method, mainly contain following 3 kinds: 1. extraction nicotine; 2. Salanesol is extracted; 3. protein tobacco is extracted.The people such as 2010 Nian Li armies mention in " tobacco waste research on utilization " literary composition, containing Phytin (inositol hexaphosphate calcium magnesium) material in tobacco waste, the Tobacco Root on the tobacco leaf planting in great Ying Jie town, inhabitants of Yuxi City in Yunnan Province ground, stem, leaf, flower part Phytin content are measured, find that its content reaches 1.0 % ~ 5.0 %, Phytin is of many uses, is applied to medication chemistry, food, daily-use chemical industry and other industry.In recent years, the demand of pharmaceutical industries to Phytin increases sharply, and world market is comparatively active.But less about the Phytin extraction process report in tobacco waste at present, be therefore optimized Phytin extraction process, the utilization ratio improving tobacco waste has comparatively actual meaning.
Report the extraction process of Phytin in corn steep liquor, Pericarppium arachidis hypogaeae, wheat bran, vinasse and rice bran both at home and abroad, corresponding extracting method comprises acid and puies forward alkali neutralization, ion-exchange, macroporous resin wash-out, microwave-assisted and ultrasonic wave acid leaching extraction etc.; Above method has certain suitability, but also there is many problems, limit extraction and the utilization of Phytin, particular case is as follows: 1. the industrial diluted acid extraction alkali moderate water-cut stage that generally adopts prepares Phytin, this method production technique is simple, easy handling, but often process 1 ton of raw material needs sewage effluent 6 ~ 7 tons, often produce 1 ton of Phytin waste discharge amount up to 60 ~ 70 tons, environmental pollution is comparatively serious; 2. ion exchange method (CN 102702250 A) adopts the phytic acid in ion exchange column absorption corn steep liquor, and then take off with pickling, liming is neutralized to pH4.0 ~ 6.0, and precipitation is dried, and pulverizes and obtains Phytin.This method is simple to operate, but output is lower, and pickling takes off the infringement of ion-exchange material comparatively large, need change resin material at any time, improve production cost.2. microwave loss mechanisms (CN200710170689.2) can shorten the production time, reduces the energy and solvent consumption, but processing condition required by microwave extraction are higher, and leaching process is more loaded down with trivial details, cannot amplify pilot scale; 3. ultrasonic extraction can improve leaching yield, save energy, and avoids high temperature on the impact of extracting composition, but ultra-sonic generator manufacturing cost is higher, easily damages, and is not suitable for large-scale commercial production.For above Problems existing, carry in alkali and extracting method based on acid, first Study on extraction is carried out to the nicotine in cigar mill of Yunnan Yuxi tobacco waste and Phytin composition, by acid leaching liquor recycle, ensureing under the precondition that extraction yield does not reduce, greatly reduce sewage discharge, reduce environmental pollution.
Summary of the invention
The object of this invention is to provide the extraction process that a kind of tobacco waste extracts inositol hexaphosphate calcium magnesium coproduction nicotine, the method production cost is low, the utilization ratio of low stain, tobacco waste is high.
The concrete operation step of the inventive method is as follows:
1, nicotine extracts
(1) collect tobacco grower to gather cigarette root, remaining tobacco leaf, cigarette stalk or fireworks after tobacco leaf, be crushed to the tobacco particle that length is less than 3 mm respectively, for subsequent use;
(2) the tobacco particle of 100 ~ 200kg is got, be placed in fermentation vat, add the hot water 300 ~ 600kg of 60 ~ 70 DEG C, mixing, regulate mixture pH to be 5.0 ~ 6.0 with the industrial sulphuric acid that mass percent concentration is 90%, soak 3 ~ 4h, soaking temperature keeps 60 ~ 70 DEG C therebetween, it is 5.0 ~ 6.0 that acid adding keeps soaking pH, stirs once every 10 ~ 15min; Then pass into water vapor, soaking temperature risen to 85 ~ 90 DEG C and remain unchanged, maintain pH5.0 ~ 6.0 constant, extract 1 ~ 1.5h, filter, filtrate is for subsequent use, is that raw material repeats above operation steps with filter residue, carry out second extraction, merge extracted twice filtrate, filter residue is for subsequent use; Abundant stirring filtrate, adjusts pH to be 6.0 ~ 7.0, cooling;
(3) in step (2) filtrate, add chloroform to extract, add-on is 100 ~ 150 kg, and get extraction phase and reclaim chloroform, obtain nicotine sulfate, extracting phase is for subsequent use;
2, Phytin (inositol hexaphosphate calcium magnesium) extracts
(1) one leaching: after extraction nicotine, gained extracting phase and filter residue merge, three immersion liquid added water or add in subsequent technique, solid-liquid mass ratio is 1:3 ~ 1:5, abundant stirring, acid adding regulates mixture pH be 2.0 ~ 3.0 and remain unchanged, maintaining extraction temperature is 25 ~ 30 DEG C, lixiviate 2 ~ 3h, stirs once every 10 ~ 15min;
(2) two leachings: step (1) mixture filters, and filtrate is that an immersion liquid is for subsequent use, and filter residue mixes with water or three immersion liquid, and repeating step (1) processing condition, carry out secondary lixiviate, filter and obtain two immersion liquid;
(3) production of inositol hexaphosphate calcium magnesium (Phytin) a: immersion liquid and two immersion liquid are merged, be that 10 % ~ 15 % calcium hydroxides adjust pH to be 4.0 ~ 4.5 with mass percent concentration, stir 10 ~ 15 min, with mass percent concentration be in the sodium hydroxide of 10 % ~ 15 % and pH value be 6.5 ~ 7.0, abundant stirring, leave standstill, taking precipitate is dried and is namely obtained inositol hexaphosphate calcium magnesium, and supernatant liquor is used for producing calcium sulfate;
(4) three leachings: two leaching gained filter residues are placed in lixiviate pond, add clear water to soak, solid-liquid mass ratio is 1:2 ~ 1:3, lixiviate 12 ~ 15h, stirs once every 30 ~ 60min, filters, obtain three immersion liquid and three leaching slags, three immersion liquid are for subsequent use, are mainly used to a supplementary leaching and water is taken in two lixiviates, and three soak the extraction that slags are used for doing feed or Salanesol.
Advantage of the present invention and technique effect as follows:
1, nicotine can first extract by the inventive method (pH5.0 ~ 6.0) under slightly acidic condition, and phytic acid can not dissociate out under this condition, continue to adjust pH to be 2.0 ~ 3.0, phytic acid can be extracted, further generation inositol hexaphosphate calcium magnesium, the maximum advantage of this technique is by continuous setup pH value, and synchronous production inositol hexaphosphate calcium magnesium and nicotine, reduce production cost.In addition, protein content in tobacco waste higher (being greater than 10 %), in nicotine and phytic acid leaching process, protein all may therefrom leach, this technology utilization sulfuric acid regulates vat liquor pH aobvious acid, recycling caustic soda soln regulates filtrate pH aobvious neutral, generates sodium sulfate salt, can make albumen passivation in this process, avoid the co-precipitation of albumen, improve product quality; After extraction nicotine and Phytin, comparatively normal diet acidity is high for the feed produced of filter residue, and palatability is strong, can improve pepsic activity, delay the residence time of protein in stomach, be beneficial to the absorption of protein, thus improves the utilization ratio of tobacco waste;
2, first the Phytin extraction process in tobacco waste is reported; After extraction nicotine adopts sulphur acid for adjusting pH to 2.0 ~ 3.0, continue to extract Phytin, manufacturing cost reduces greatly; By the recycle of part vat liquor, decrease environmental pollution;
3, this technique extraction efficiency is high, can synchronously obtain Phytin and nicotine, greatly reduce the discharge of sewage, reduces production cost, has comparatively actual meaning for making full use of tobacco waste resource.
Embodiment
Below by embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited to described content.
embodiment 1:this tobacco waste extracts the extracting method of inositol hexaphosphate calcium magnesium coproduction nicotine, and concrete operations are as follows:
(1) collect tobacco grower's cigarette root after tobacco leaf of gathering to be crushed to length and to be less than 3 mm, diameter is less than the cigarette root particle of 1mm;
(2) get the cigarette root particle of 100kg, be placed in fermentation vat, add the hot water 300kg of 65 DEG C, adjust pH to be 5.0 with the industrial sulphuric acid that mass percent concentration is 90%, soaking temperature keeps 65 DEG C therebetween, and it is 5.0 that acid adding keeps soaking pH, stir once every 10min, soak 3h, then pass into water vapor, soaking temperature risen to 85 DEG C and remain unchanged, maintain pH5.0 constant, extract 1h, filter, filtrate is for subsequent use; Be that raw material repeats above operation steps with filter residue, carry out second extraction, merge extracted twice filtrate, filter residue is for subsequent use; Abundant stirring filtrate, adjusts pH to be 7.0, cooling;
(3) in the filtrate after neutralization, add chloroform extraction, add-on is 100 kg, and get extraction phase and reclaim chloroform, obtain nicotine sulfate, extracting phase is for subsequent use;
(4) after extracting nicotine, gained extracting phase and filter residue merge, and add water, keep solid-liquid mass ratio to be 1:3, abundant stirring, adjust pH be 2.0 and remain unchanged with the industrial sulphuric acid that mass percent concentration is 90%, extraction temperature is 25 DEG C, lixiviate 3h, stirs once every 15min;
(5) filter, filtrate is that an immersion liquid is for subsequent use, and filter residue mixes with water, and repeating step (4) processing condition, carry out secondary lixiviate, filters and obtains two immersion liquid;
(6) immersion liquid and two immersion liquid are merged, pH is adjusted to be 4.0 with the calcium hydroxide that mass percent concentration is 10 %, stir 10 min, 7.0 are neutralized to the sodium hydroxide that mass percent concentration is 10 %, abundant stirring, leave standstill, taking precipitate is dried and is namely obtained inositol hexaphosphate calcium magnesium, and supernatant liquor is used for producing calcium sulfate;
(7) two leaching gained filter residues are placed in lixiviate pond, add clear water to soak, solid-liquid mass ratio is kept to be 1:2, stir once every 30min, lixiviate 12h, filter, obtain three immersion liquid and three leaching slags, three immersion liquid are for subsequent use, are mainly used to take water as a leaching supplementary in extraction next time and two lixiviates, and three soak the extraction that slags are used for doing feed or Salanesol.
The nicotine purity obtained in the present embodiment is 65%, and reach 98% by refining purity further, nicotine extraction yield is 79%; The purity of gained inositol hexaphosphate calcium magnesium is 80%, and extraction yield is 4%.
embodiment 2:this tobacco waste extracts the extracting method of inositol hexaphosphate calcium magnesium coproduction nicotine, and concrete operations are as follows:
(1) collect tobacco grower's cigarette stalk after tobacco leaf of gathering to be crushed to length and to be less than 3 mm, diameter is less than the cigarette stalk particle of 1mm;
(2) get the cigarette stalk particle of 100kg, be placed in fermentation vat, add the hot water 350kg of 70 DEG C, industrial sulphuric acid with 90% adjusts pH to be 5.2, and soaking temperature keeps 70 DEG C therebetween, and it is 5.2 that acid adding keeps soaking pH, stir once every 10min, soak 3h, then pass into water vapor, soaking temperature risen to 85 DEG C and remain unchanged, maintain pH5.2 constant, extract 1h, filter, filtrate is for subsequent use; Be that raw material repeats above operation steps with filter residue, carry out second extraction, merge extracted twice filtrate, filter residue is for subsequent use; Abundant stirring filtrate, adjusts pH to be 7.0, cooling;
(3) in the filtrate after neutralization, add chloroform extraction, add-on is 120 kg, and get extraction phase and reclaim chloroform, obtain nicotine sulfate, extracting phase is for subsequent use;
(4) after extracting nicotine, gained extracting phase and filter residue merge, add three immersion liquid produced in embodiment 1, solid-liquid mass ratio is kept to be 1:3, abundant stirring, pH is adjusted to be 2.5 and to remain unchanged with the industrial sulphuric acid that mass percent concentration is 90%, extraction temperature is 25 DEG C, lixiviate 3h, stirs once every 15min;
(5) filter, filtrate is that an immersion liquid is for subsequent use, and filter residue mixes with three immersion liquid produced in embodiment 1, and repeating step (4) processing condition, carry out secondary lixiviate, filters and obtains two immersion liquid;
(6) immersion liquid and two immersion liquid are merged, pH is adjusted to be 4.0 with the calcium hydroxide that mass percent concentration is 10 %, stir 10 min, 7.0 are neutralized to the sodium hydroxide that mass percent concentration is 10 %, abundant stirring, leave standstill, taking precipitate is dried and is namely obtained inositol hexaphosphate calcium magnesium, and supernatant liquor is used for producing calcium sulfate;
(7) two leaching gained filter residues are placed in lixiviate pond, add clear water to soak, solid-liquid mass ratio is kept to be 1:2, stir once every 30min, lixiviate 12h, filter, obtain three immersion liquid and three leaching slags, three immersion liquid are for subsequent use, are mainly used to take water as a leaching supplementary in extraction next time and two lixiviates, and three soak the extraction that slags are used for doing feed or Salanesol.
The nicotine purity obtained in the present embodiment is 60%, and reach 96% by refining purity further, nicotine extraction yield is 75%; Gained inositol hexaphosphate calcium magnesium purity is 77%, and extraction yield is 2%.
embodiment 3:this tobacco waste extracts the extracting method of inositol hexaphosphate calcium magnesium coproduction nicotine, and concrete operations are as follows:
(1) collect tobacco grower's remaining tobacco leaf powder after tobacco leaf of gathering and be broken to the tobacco leaf particle that length is less than 3 mm;
(2) get the tobacco leaf particle of 150kg, be placed in fermentation vat, add the hot water 500kg of 65 DEG C, industrial sulphuric acid with 90% adjusts pH to be 6.0, and soaking temperature keeps 65 DEG C therebetween, and it is 6.0 that acid adding keeps soaking pH, stir once every 15min, soak 3.5h, then pass into steam, soaking temperature risen to 90 DEG C and remain unchanged, maintain pH 6.0 constant, extract 1.5h, filter, filtrate is for subsequent use; Be that raw material repeats above operation steps with filter residue, carry out second extraction, merge extracted twice filtrate, filter residue is for subsequent use; Abundant stirring filtrate, adjusts pH to be 6.0, cooling;
(3) in the filtrate after neutralization, add chloroform extraction, add-on is 120kg, and get extraction phase and reclaim chloroform, obtain nicotine sulfate, extracting phase is for subsequent use;
(4) after extracting nicotine, gained extracting phase and filter residue merge, and add water or three immersion liquid, keep solid-liquid mass ratio to be 1:4, abundant stirring, adjust pH be 2.0 and remain unchanged with the industrial sulphuric acid that mass percent concentration is 90%, extraction temperature is 25 DEG C, lixiviate 2h, stirs once every 12min;
(5) filter, filtrate is that an immersion liquid is for subsequent use, and three immersion liquid that filter residue produces with embodiment 2 mix, and repeating step (4) processing condition, carry out secondary lixiviate, filters and obtains two immersion liquid;
(6) immersion liquid and two immersion liquid are merged, pH is adjusted to be 4.5 with the calcium hydroxide that mass percent concentration is 15%, stir 15 min, being neutralized to pH with the sodium hydroxide that mass percent concentration is 15 % is 6.5, abundant stirring, leave standstill, taking precipitate is dried and is namely obtained inositol hexaphosphate calcium magnesium, and supernatant liquor is used for producing calcium sulfate;
(7) two leaching gained filter residues are placed in lixiviate pond, add clear water to soak, solid-liquid mass ratio is kept to be 1:3, stir once every 40min, lixiviate 13h, filter, obtain three immersion liquid and three leaching slags, three immersion liquid are for subsequent use, are mainly used to take water as a leaching supplementary in extraction next time and two lixiviates, and three soak the extraction that slags are used for doing feed or Salanesol.
The nicotine purity obtained in the present embodiment is 58%, and reach 97% by refining purity further, nicotine extraction yield is 78%; The purity of gained inositol hexaphosphate calcium magnesium is 79%, and extraction yield is 3%.
embodiment 4:this tobacco waste extracts the extracting method of inositol hexaphosphate calcium magnesium coproduction nicotine, and concrete operations are as follows:
(1) collect tobacco grower's fireworks after tobacco leaf of gathering and be crushed to the fireworks particle that length is less than 3 mm;
(2) get the fireworks particle of 200kg, be placed in fermentation vat, add the hot water 600kg of 60 DEG C, adjust pH to be 5.5 with the industrial sulphuric acid that mass percent concentration is 90%, soaking temperature keeps 60 DEG C therebetween, and it is 5.5 that acid adding keeps soaking pH, stir once every 12min, soak 4h, then pass into water vapor, soaking temperature risen to 88 DEG C and remain unchanged, maintain pH5.5 constant, extract 1.4h, filter, filtrate is for subsequent use; Be that raw material repeats above operation steps with filter residue, carry out second extraction, merge extracted twice filtrate, filter residue is for subsequent use; Abundant stirring filtrate, adjusts pH to be 6.5, cooling;
(3) in the filtrate after neutralization, add chloroform extraction, add-on is 150 kg, and get extraction phase and reclaim chloroform, obtain nicotine sulfate, extracting phase is for subsequent use;
(4) after extracting nicotine, gained extracting phase and filter residue merge, and add water, keep solid-liquid mass ratio to be 1:5, abundant stirring, adjust pH be 3.0 and remain unchanged with the industrial sulphuric acid that mass percent concentration is 90%, extraction temperature is 30 DEG C, lixiviate 2.5h, stirs once every 10min;
(5) filter, filtrate is that an immersion liquid is for subsequent use, and filter residue mixes with water, and repeating step (4) processing condition, carry out secondary lixiviate, filters and obtains two immersion liquid;
(6) immersion liquid and two immersion liquid are merged, pH is adjusted to be 4.0 with the calcium hydroxide that mass percent concentration is 12 %, stir 12 min, 7.0 are neutralized to the sodium hydroxide that mass percent concentration is 10 %, abundant stirring, leave standstill, taking precipitate is dried and is namely obtained inositol hexaphosphate calcium magnesium, and supernatant liquor is used for producing calcium sulfate;
(7) two leaching gained filter residues are placed in lixiviate pond, add clear water to soak, solid-liquid mass ratio is kept to be 1:2.5, stir once every 60min, lixiviate 15h, filter, obtain three immersion liquid and three leaching slags, three immersion liquid are for subsequent use, are mainly used to take water as a leaching supplementary in extraction next time and two lixiviates, and three soak the extraction that slags are used for doing feed or Salanesol.
The nicotine purity obtained in the present embodiment is 50%, and reach 98% by refining purity further, nicotine extraction yield is 48%; Obtain inositol hexaphosphate calcium magnesium purity be 65%, extraction yield is 1.8%.
Claims (1)
1. tobacco waste extracts an extracting method for inositol hexaphosphate calcium magnesium coproduction nicotine, it is characterized in that carrying out as follows:
A, extraction nicotine
(1) collect cigarette root, remaining tobacco leaf, cigarette stalk or the fireworks of gathering after tobacco leaf, pulverize as length is less than the tobacco particle of 3 mm respectively, for subsequent use;
(2) the tobacco particle getting 100 ~ 200 kg adds in the hot water 300 ~ 600kg of 60 ~ 70 DEG C and mixes, regulate mixture pH to be 5.0 ~ 6.0, soak 3 ~ 4h, soaking temperature keeps 60 ~ 70 DEG C, it is 5.0 ~ 6.0 that acid adding keeps soaking pH, stirs once every 10 ~ 15min; Pass into water vapor, soaking temperature risen to 85 ~ 90 DEG C and remain unchanged, maintain pH5.0 ~ 6.0 constant, extract 1 ~ 1.5h, filter, filtrate is for subsequent use; Getting filter residue is that raw material repeats above operation steps, carries out second extraction, and merge the filtrate of extracted twice, filter residue is for subsequent use; Abundant stirring filtrate, adjusts pH to be 6.0 ~ 7.0, cooling;
(3) in step (2) filtrate, add chloroform to extract, add-on is 100 ~ 150 kg, and get extraction phase and reclaim chloroform, obtain nicotine sulfate, extracting phase is for subsequent use;
B, inositol hexaphosphate calcium magnesium extract
(1) one leaching: after extraction nicotine, gained extracting phase and filter residue merge, three immersion liquid added water or add in subsequent technique, solid-liquid mass ratio is 1:3 ~ 1:5, abundant stirring, mixture pH is regulated to be 2.0 ~ 3.0 and to remain unchanged, maintaining extraction temperature is 25 ~ 30 DEG C, lixiviate 2 ~ 3h, stirs once every 10 ~ 15min;
(2) two leachings: mixture filters, and filtrate is that an immersion liquid is for subsequent use, and filter residue mixes with water or three immersion liquid, and the processing condition of repeating step (1), carry out secondary lixiviate, filter and obtain two immersion liquid;
(3) production of inositol hexaphosphate calcium magnesium a: immersion liquid and two immersion liquid are merged, pH is adjusted to be 4.0 ~ 4.5 with the calcium hydroxide that mass percent concentration is 10 % ~ 15 %, stir 10 ~ 15 min, with mass percent concentration be in the sodium hydroxide of 10 % ~ 15 % and pH value be 6.5 ~ 7.0, abundant stirring, leave standstill, taking precipitate is dried and is namely obtained inositol hexaphosphate calcium magnesium, and supernatant liquor is used for producing calcium sulfate;
(4) three leachings: two leaching gained filter residues are placed in lixiviate pond, add clear water to soak, solid-liquid mass ratio is 1:2 ~ 1:3, lixiviate 12 ~ 15h, stirs once every 30 ~ 60min, filters, obtain three immersion liquid and three leaching slags, three immersion liquid are for subsequent use, are mainly used to a supplementary leaching and water is taken in two lixiviates, and three leaching slags are as feed or the extraction of Salanesol;
Wherein regulate mixture ph with the industrial sulphuric acid that mass percent concentration is 90%.
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