CN105002225A - Method for preparing 4-ethenyl guaiacol by utilizing bagasse - Google Patents
Method for preparing 4-ethenyl guaiacol by utilizing bagasse Download PDFInfo
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- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
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Abstract
The invention discloses a method for preparing 4-ethenyl guaiacol by utilizing bagasse, and belongs to the technical field of bioengineering. According to the method, the 4-ethenyl guaiacol is prepared through the steps of drying the bagasse, adding sulfuric acid and stirring, filtering, blowing up, cooling, then mixing with natural ferulic acid and loading into a chitling, soaking with a nutrient solution, oxygenating, feeding into an extruding machine for extruding, fermenting, filtering, performing ethyl acetate extraction and carrying out vacuum evaporation. The method provided by the invention has the beneficial effects that the purity of the 4-ethenyl guaiacol prepared by using the method reaches above 97 percent, the cost is reduced by 20 to 30 percent in comparison with that of a traditional method, environmental pollution is less, by-products are less, the yield is high, the operation is simple, the production environment is friendly, safety and reliability are realized, the bagasse is sufficiently utilized for preparing the 4-ethenyl guaiacol, so that the sustainable utilization of resources is realized, the material is easy to obtain, the resources are wide, and the industrialization is easy to realize; the method is an economical and effective method for producing the 4-ethenyl guaiacol and has an extraordinary industrial prospect.
Description
Technical field
The present invention relates to a kind of method utilizing bagasse to prepare 4-vinyl guaiacol, belong to technical field of bioengineering.
Background technology
4-vinyl guaiacol has another name called 2-methoxyl-4-vinyl phenol, to vinyl guaiacol, molecular formula is C9H10O2, and molecular weight is 150.18, is colourless or flaxen oily liquids, slightly sweet taste, in fermentation fragrance.4-VG is a kind of phenol compounds material that can produce peat-reek or cloves class fragrance, and its threshold of feelings is very low, is only 0.3mg/L, and it can improve the organoleptic quality of food, has a significant impact the natural fragrance of the food such as drinks, soy sauce, cheese, beverage.4-VG is a kind of conventional high-grade spices, is mainly used in food to increase its fragrance ingredient, also for industries such as tobacco, daily use chemicals, medicine, essence synthesis.At liquor industry, 4-VG is with requisite fragrance matter in the wheat class top fermented beer that is supplementary material, is also a kind of important flavour substances in Maotai-flavor liquor and grape wine.
Current chemical synthesis is the method for conventional production 4-VG, as Chinese patent literature CN 101885669 A discloses " a kind of preparation method of 4-vinyl guaiacol ", first in reactor, quinoline, forulic acid and the Resorcinol as stopper is dropped into successively, heating, when temperature is elevated to 180-185 DEG C, reaction 4-5 hours; Add solvent benzol by above-mentioned reaction solution, and add hydrochloric acid, stir, stratification, till detection aqueous pH values is neutrality, finally add siccative Calcium Chloride Powder Anhydrous; Again dried solution is put into distiller, the benzene as solvent steams by normal pressure, is steamed by product, can pack commercially available under then connecting the gas phase temperature of upper vacuum pump below 100 DEG C.But the environmental issue that chemical synthesis ubiquity is severeer, reaction conditions is generally comparatively violent, higher to equipment requirements, complex manufacturing, and product yield is low; And due to the residue containing materials such as raw material, by product, solvents in product, the 4-VG that therefore the method obtains cannot directly add in food.
Bagasse is that sugarcane is through the broken fibering residue with squeezing after sugarcane juice, it is the principal by product of sugar industry, bagasse with Mierocrystalline cellulose, hemicellulose and xylogen for main component, also containing a small amount of ash content, protein, pectin and fat, China's year sugarcane yield about 1.23 hundred million tons, bagasse at least accounts for sugarcane quality 10% ~ 15%, by generation more than 1,230 ten thousand tons bagasse.
Summary of the invention
Technical problem to be solved by this invention: the drawback complicated for chemical method synthesis 4-vinyl guaiacol operational path, yield is low, environmental pollution is large, by product is many, provide a kind of side utilizing bagasse to prepare 4-vinyl guaiacol, having that raw material sources are extensive, by product is few, product yield is high, production cost is low, be easy to realize industrialized feature, is the 4-vinyl guaiacol production method that there is industrialization prospect a kind of economical and effective and pole.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be: a kind of method utilizing bagasse to prepare 4-vinyl guaiacol, and its concrete preparation process is:
(1) get bagasse to put into air-drying box and carry out air-dry, ensure that the water content in bagasse is 5 ~ 8%, again bagasse is put into container, add the sulphuric acid soln that massfraction is 10 ~ 15% wherein, its add-on is that every gram of bagasse adds 2.5mL sulphuric acid soln, stir 7 ~ 10h, temperature is set as 35 ~ 40 DEG C, filters;
(2) bagasse after above-mentioned filtration is put into steam to expose to the sun brokenly instrument borehole blasting 2 ~ 4min, pressure setting is 1.7 ~ 2.2MPa, and temperature is set as 200 ~ 220 DEG C, is taken out by the bagasse after explosion, is cooled to 1 ~ 4 DEG C;
(3) fresh chitling is got, with clear water, chitling outside surface is cleaned, chitling inside does not need cleaning, the ratio of 6:1 in mass ratio, mixes the bagasse obtained by step (2) with natural ferulaic acid, is loaded in chitling again, chitling two ends do not need sealing, chitling is put into nutritive medium soak 4 ~ 6 days, keep temperature to be 30 ~ 35 DEG C, in immersion process, every 5 ~ 8h uses oxygenating machine to carry out oxygenating 15 ~ 20min to nutritive medium;
(4) inner for chitling bagasse is extruded by the chitling forcing machine after middle for step (3) immersion, put into above-mentioned nutritive medium, add the feruloyl esterase of the cellulase of 1 ~ 1.8% of bagasse quality and 2 ~ 3% of bagasse quality more wherein, be 32 ~ 36 DEG C in temperature, rotating speed is under 160 ~ 200r/min, ferments 3 ~ 6 days, then aperture is used to be 0.01 ~ 0.12 μm of millipore filtration, under operating pressure is 0.07 ~ 1.2MPa, filter, obtain fermented liquid;
(5) fermented liquid of gained in step (4) is put into container, stir according to adding n-butyl acetate extraction agent with fermentating liquid volume than 1:5 again, leave standstill 20 ~ 25min, phase-splitting obtains the extraction phase of 4-vinyl guaiacol, by the extraction agent vacuum-evaporation in extraction phase, 4-vinyl guaiacol product can be obtained.
Described step (3) Middle nutrition liquid counts 75 ~ 80% water, 5 ~ 7% glucose, 7 ~ 9% peptones and 8 ~ 9% sodium-chlor by percent mass, mixed.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the 4-vinyl guaiacol environmental pollution that the method is obtained is little, by product is few, yield is high, simple to operate, Product environment is friendly, safe and reliable;
(2) make full use of bagasse and prepare 4-vinyl guaiacol, achieve the sustainable use of resource, material is easy to get, wide material sources;
(3) the 4-vinyl guaiacol purity that the present invention obtains reaches more than 97%, and cost reduces 20 ~ 30% than traditional method.
Embodiment
First get bagasse to put into air-drying box and carry out air-dry, ensure that the water content in bagasse is 5 ~ 8%, again bagasse is put into container, add the sulphuric acid soln that massfraction is 10 ~ 15% wherein, its add-on is that every gram of bagasse adds 2.5mL sulphuric acid soln, stir 7 ~ 10h, temperature is set as 35 ~ 40 DEG C, filters; Bagasse after above-mentioned filtration is put into steam to expose to the sun brokenly instrument borehole blasting 2 ~ 4min, pressure setting is 1.7 ~ 2.2MPa, and temperature is set as 200 ~ 220 DEG C, is taken out by the bagasse after explosion, is cooled to 1 ~ 4 DEG C; Get fresh chitling, with clear water, chitling outside surface is cleaned, chitling inside does not need cleaning, the ratio of 6:1 in mass ratio again, mixes above-mentioned obtained bagasse with natural ferulaic acid, in loading chitling, chitling two ends do not need sealing, chitling is put into nutritive medium soak 4 ~ 6 days, keep temperature to be 30 ~ 35 DEG C, in immersion process, every 5 ~ 8h uses oxygenating machine to carry out oxygenating 15 ~ 20min to nutritive medium; Inner for chitling bagasse is extruded by the chitling forcing machine after above-mentioned immersion being completed again, put into above-mentioned nutritive medium, add the feruloyl esterase of the cellulase of 1 ~ 1.8% of bagasse quality and 2 ~ 3% of bagasse quality more wherein, be 32 ~ 36 DEG C in temperature, rotating speed is under 160 ~ 200r/min, ferments 3 ~ 6 days, then aperture is used to be 0.01 ~ 0.12 μm of millipore filtration, under operating pressure is 0.07 ~ 1.2MPa, filter, obtain fermented liquid; Finally the fermented liquid of above-mentioned gained is put into container, stir according to adding n-butyl acetate extraction agent with fermentating liquid volume than 1:5 again, leave standstill 20 ~ 25min, phase-splitting obtains the extraction phase of 4-vinyl guaiacol, by the extraction agent vacuum-evaporation in extraction phase, 4-vinyl guaiacol product can be obtained; Described nutritive medium counts 75 ~ 80% water, 5 ~ 7% glucose, 7 ~ 9% peptones and 8 ~ 9% sodium-chlor by percent mass, mixed.
Example 1
First get bagasse to put into air-drying box and carry out air-dry, ensure that the water content in bagasse is 5%, then bagasse is put into container, add the sulphuric acid soln that massfraction is 10% wherein, its add-on is that every gram of bagasse adds 2.5mL sulphuric acid soln, stirs 7h, temperature is set as 35 DEG C, filters; Bagasse after above-mentioned filtration is put into steam to expose to the sun brokenly instrument borehole blasting 2min, pressure setting is 1.7MPa, and temperature is set as 200 DEG C, is taken out by the bagasse after explosion, is cooled to 1 DEG C; Get fresh chitling, with clear water, chitling outside surface is cleaned, chitling inside does not need cleaning, the ratio of 6:1 in mass ratio again, mixes above-mentioned obtained bagasse with natural ferulaic acid, in loading chitling, chitling two ends do not need sealing, chitling is put into nutritive medium soak 4 days, keep temperature to be 30 DEG C, in immersion process, every 5h uses oxygenating machine to carry out oxygenating 15min to nutritive medium; Inner for chitling bagasse is extruded by the chitling forcing machine after above-mentioned immersion being completed again, put into above-mentioned nutritive medium, add the feruloyl esterase of the cellulase of 1% of bagasse quality and 2% of bagasse quality more wherein, be 32 DEG C in temperature, rotating speed is under 160r/min, ferments 3 days, then aperture is used to be 0.01 μm of millipore filtration, under operating pressure is 0.07MPa, filter, obtain fermented liquid; Finally the fermented liquid of above-mentioned gained is put into container, stir according to adding n-butyl acetate extraction agent with fermentating liquid volume than 1:5 again, leave standstill 20min, phase-splitting obtains the extraction phase of 4-vinyl guaiacol, by the extraction agent vacuum-evaporation in extraction phase, 4-vinyl guaiacol product can be obtained; Described nutritive medium is 79g water, 6g glucose, 7g peptone and 8g sodium-chlor by total mass 100g, mixed.
The 4-vinyl guaiacol purity detected obtained by the invention described above is 97%, and cost reduces 20% than traditional method.
Example 2
First get bagasse to put into air-drying box and carry out air-dry, ensure that the water content in bagasse is 7%, again bagasse is put into container, add the sulphuric acid soln that massfraction is 12% wherein, its add-on is that every gram of bagasse adds 2.5mL sulphuric acid soln, stir 8.5h, temperature is set as 38 DEG C, filters; Bagasse after above-mentioned filtration is put into steam to expose to the sun brokenly instrument borehole blasting 3min, pressure setting is 1.9MPa, and temperature is set as 210 DEG C, is taken out by the bagasse after explosion, is cooled to 2 DEG C; Get fresh chitling, with clear water, chitling outside surface is cleaned, chitling inside does not need cleaning, the ratio of 6:1 in mass ratio again, mixes above-mentioned obtained bagasse with natural ferulaic acid, in loading chitling, chitling two ends do not need sealing, chitling is put into nutritive medium soak 5 days, keep temperature to be 33 DEG C, in immersion process, every 6.5h uses oxygenating machine to carry out oxygenating 17min to nutritive medium; Inner for chitling bagasse is extruded by the chitling forcing machine after above-mentioned immersion being completed again, put into above-mentioned nutritive medium, add the feruloyl esterase of the cellulase of 1.4% of bagasse quality and 2.5% of bagasse quality more wherein, be 34 DEG C in temperature, rotating speed is under 180r/min, ferments 5 days, then aperture is used to be 0.06 μm of millipore filtration, under operating pressure is 0.09MPa, filter, obtain fermented liquid; Finally the fermented liquid of above-mentioned gained is put into container, stir according to adding n-butyl acetate extraction agent with fermentating liquid volume than 1:5 again, leave standstill 22min, phase-splitting obtains the extraction phase of 4-vinyl guaiacol, by the extraction agent vacuum-evaporation in extraction phase, 4-vinyl guaiacol product can be obtained; Described nutritive medium is 75g water, 7g glucose, 9g peptone and 9g sodium-chlor by total mass 100g, mixed.
The 4-vinyl guaiacol purity detected obtained by the invention described above is 98.2%, and cost reduces 25% than traditional method.
Example 3
First get bagasse to put into air-drying box and carry out air-dry, ensure that the water content in bagasse is 8%, again bagasse is put into container, add the sulphuric acid soln that massfraction is 15% wherein, its add-on is that every gram of bagasse adds 2.5mL sulphuric acid soln, stir 10h, temperature is set as 40 DEG C, filters; Bagasse after above-mentioned filtration is put into steam to expose to the sun brokenly instrument borehole blasting 4min, pressure setting is 2.2MPa, and temperature is set as 220 DEG C, is taken out by the bagasse after explosion, is cooled to 4 DEG C; Get fresh chitling, with clear water, chitling outside surface is cleaned, chitling inside does not need cleaning, the ratio of 6:1 in mass ratio again, mixes above-mentioned obtained bagasse with natural ferulaic acid, in loading chitling, chitling two ends do not need sealing, chitling is put into nutritive medium soak 6 days, keep temperature to be 35 DEG C, in immersion process, every 8h uses oxygenating machine to carry out oxygenating 20min to nutritive medium; Inner for chitling bagasse is extruded by the chitling forcing machine after above-mentioned immersion being completed again, put into above-mentioned nutritive medium, add the feruloyl esterase of the cellulase of 1.8% of bagasse quality and 3% of bagasse quality more wherein, be 36 DEG C in temperature, rotating speed is under 200r/min, ferments 6 days, then aperture is used to be 0.12 μm of millipore filtration, under operating pressure is 1.2MPa, filter, obtain fermented liquid; Finally the fermented liquid of above-mentioned gained is put into container, stir according to adding n-butyl acetate extraction agent with fermentating liquid volume than 1:5 again, leave standstill 25min, phase-splitting obtains the extraction phase of 4-vinyl guaiacol, by the extraction agent vacuum-evaporation in extraction phase, 4-vinyl guaiacol product can be obtained; Described nutritive medium is 80g water, 5g glucose, 7g peptone and 8g sodium-chlor by total mass 100g, mixed.
The 4-vinyl guaiacol purity detected obtained by the invention described above is 99.1%, and cost reduces 30% than traditional method.
Claims (2)
1. utilize bagasse to prepare a method for 4-vinyl guaiacol, it is characterized in that concrete preparation process is:
Get bagasse to put into air-drying box and carry out air-dry, ensure that the water content in bagasse is 5 ~ 8%, again bagasse is put into container, add the sulphuric acid soln that massfraction is 10 ~ 15% wherein, its add-on is that every gram of bagasse adds 2.5mL sulphuric acid soln, stir 7 ~ 10h, temperature is set as 35 ~ 40 DEG C, filters;
Bagasse after above-mentioned filtration is put into steam to expose to the sun brokenly instrument borehole blasting 2 ~ 4min, pressure setting is 1.7 ~ 2.2MPa, and temperature is set as 200 ~ 220 DEG C, is taken out by the bagasse after explosion, is cooled to 1 ~ 4 DEG C;
Get fresh chitling, with clear water, chitling outside surface is cleaned, chitling inside does not need cleaning, the ratio of 6:1 in mass ratio, mixes the bagasse obtained by step (2) with natural ferulaic acid, is loaded in chitling again, chitling two ends do not need sealing, chitling is put into nutritive medium soak 4 ~ 6 days, keep temperature to be 30 ~ 35 DEG C, in immersion process, every 5 ~ 8h uses oxygenating machine to carry out oxygenating 15 ~ 20min to nutritive medium;
Inner for chitling bagasse is extruded by the chitling forcing machine after having soaked in step (3), put into above-mentioned nutritive medium, add the feruloyl esterase of the cellulase of 1 ~ 1.8% of bagasse quality and 2 ~ 3% of bagasse quality more wherein, be 32 ~ 36 DEG C in temperature, rotating speed is under 160 ~ 200r/min, ferments 3 ~ 6 days, then aperture is used to be 0.01 ~ 0.12 μm of millipore filtration, under operating pressure is 0.07 ~ 1.2MPa, filter, obtain fermented liquid;
The fermented liquid of gained in step (4) is put into container, stir according to adding n-butyl acetate extraction agent with fermentating liquid volume than 1:5 again, leave standstill 20 ~ 25min, phase-splitting obtains the extraction phase of 4-vinyl guaiacol, by the extraction agent vacuum-evaporation in extraction phase, 4-vinyl guaiacol product can be obtained.
2. a kind of method utilizing bagasse to prepare 4-vinyl guaiacol according to claim 1, it is characterized in that: described step (3) Middle nutrition liquid counts 75 ~ 80% water, 5 ~ 7% glucose, 7 ~ 9% peptones and 8 ~ 9% sodium-chlor by percent mass, mixed.
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