CN112717890A - Baked fermented plant konjac glucomannan composite porous particle, preparation method and application thereof - Google Patents
Baked fermented plant konjac glucomannan composite porous particle, preparation method and application thereof Download PDFInfo
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- CN112717890A CN112717890A CN202011413408.3A CN202011413408A CN112717890A CN 112717890 A CN112717890 A CN 112717890A CN 202011413408 A CN202011413408 A CN 202011413408A CN 112717890 A CN112717890 A CN 112717890A
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- konjac glucomannan
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/04—Tobacco smoke filters characterised by their shape or structure
- A24D3/048—Tobacco smoke filters characterised by their shape or structure containing additives
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28085—Pore diameter being more than 50 nm, i.e. macropores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28088—Pore-size distribution
Abstract
The invention discloses a baked fermented plant konjac glucomannan composite porous particle which comprises konjac glucomannan and baked fermented plant particles, wherein the mass fraction of the baked fermented plant particles is 66.7-97.2, and the mass fraction of the konjac glucomannan is 2.8-33.3. The invention also discloses a preparation method of the baked fermented plant konjac glucomannan composite porous particle and application of the baked fermented plant konjac glucomannan composite porous particle in adsorption, harm removal and flavoring of a tobacco filter stick.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a fermented baked plant konjac glucomannan composite porous particle, a preparation method and application thereof.
Background
With the increasingly prominent smoking and health problems and the increased awareness of consumers to health, low-harm cigarettes also become a necessary development trend in the tobacco industry. The method for adding the adsorbing material into the filter stick is an effective method, and a great deal of research is carried out on the adsorbing material added into the filter stick in the tobacco industry at home and abroad in recent years. The currently reported adsorbing materials for filter sticks comprise activated carbon, sepiolite, molecular sieves, zeolite, silica gel and the like. The materials such as the activated carbon, the sepiolite, the molecular sieve, the zeolite, the silica gel and the like have good effects on reducing tar and harm, but can bring about the problems of attenuation of tobacco fragrance, introduction of bad smell and the like. In order to solve the problems, the roasted and carbonized spice plant particles are directly added into the cigarette filter stick, so that the effects of adsorption and harm reduction and flavoring can be achieved. For example, in patent CN109222230A, firstly, the aromatic plant is subjected to soft carbonization at 120-200 ℃ (gaps are formed in the plant, but the fragrance characteristics of the plant are not damaged), and then the aromatic plant is fermented and crushed into particles to be added into the cigarette filter stick. Although the above patent solves the problem of adsorption, harm reduction and perfuming, the problems of large adsorption resistance, fast volatilization of fragrance and poor storage stability still exist.
Konjac Glucomannan (KGM) is an organic biomass material, is a water-soluble natural polysaccharide, and has a main chain with a tertiary structure, wherein the primary structure is a linear structure which takes glucose and mannose as repeating units and is combined according to a certain molar ratio; the secondary structure is a double-folded spiral structure presented by the KGM molecular chain through stretching; the tertiary structure is a three-dimensional structure presented by the rotation of KGM molecules in a three-dimensional space; because of its unique structure, KGM has the advantages of good cross-linking property, simple forming process, certain toughness, etc. It also has the following unique properties: a. thickening property, wherein the viscosity of the konjac powder sol with the mass fraction of 1% can reach thousands of mPa/s; b. gelling, the KGM is a non-newtonian fluid, exhibits a high viscosity at low concentrations, and gels upon standing; c. the water-retaining property, KGM contains a large amount of hydrophilic groups, so the water-retaining capacity can be 40 times higher than the self weight, and the water-retaining lubricating effect is better. KGM is an extract of the roots and tubers of Amorphophallus konjac of the Araceae family. The konjak belongs to the most species in Yunnan, has large planting amount, and has the advantages of wide raw material source, low cost, easy extraction and the like.
The invention wraps the fermented and baked plant spice by KGM gelation for the first time, and then the plant spice is used for flavoring in the tobacco filter stick, thereby obtaining better effect.
Disclosure of Invention
The invention firstly utilizes the konjac glucomannan to prepare the baked fermented plant konjac glucomannan composite porous particle added with the baked fermented plant particle, and the composite porous particle is a composite porous material with good pore structure, pore size and porosity. The baked fermented plant composite porous particles are used in tobacco, and have the advantages of small adsorption resistance, stable and uniform fragrance volatilization, good cigarette storage stability and long-term fragrance retention.
The technical scheme of the invention is as follows:
the invention discloses a baked fermented plant konjac glucomannan composite porous particle which is characterized by comprising konjac glucomannan and baked fermented plant particles, wherein the mass fraction of the baked fermented plant particles is 66.7-97.2, and the mass fraction of the konjac glucomannan is 2.8-33.3.
Preferably, the preparation steps of the baked fermented plant particles are as follows:
firstly, sealing the dried plants at 120-200 ℃ and keeping for 2-8 hours for baking treatment;
secondly, spraying the product after baking treatment in the step I to bacillus subtilis Van3, and then fermenting for 24-72 hours at the temperature of 22 ℃ and the relative humidity of 60%;
and thirdly, crushing the product obtained after the fermentation in the step II into powder with the particle size of 100-180 meshes, and then bonding the powder into particles with the particle size of 20-60 meshes by using an adhesive, namely the baked fermented plant particles.
Preferably, the plant is an aroma-containing plant, and the aroma-containing plant is one or a combination of dark plum, white snow tea, ciguatin, pu' er tea, roxburgh rose, tobacco, red snow tea, sorghum, corn, coffee, tobacco, dill seed, walnut shell, ganoderma lucidum, kudzu root, dwarf lilyturf tuber, polished round-grained rice, glutinous rice, red rice, Chinese date, fennel, sarcandra glabra, rice, damnacanthus, Broussonetia papyrifera, isatis root, vinasse and the like.
Preferably, the roasted and fermented plant konjac glucomannan composite porous particles are in a porous structure; the baked fermented plant konjac glucomannan composite porous particle takes a three-dimensional network formed by the konjac glucomannan as a frame, takes the baked fermented plant particle as a filling material, and is wrapped in the konjac glucomannan.
Preferably, the diameter of the baked fermented plant konjac glucomannan composite porous particle is 0.45mm-2mm, the porosity of the particle is 10% -85%, and the pore diameter of the particle is 0.05 μm-225 μm; the specific surface area is 0.1523m2/g-7.5482m2/g。
The second aspect of the invention discloses a preparation method of a baking fermented plant konjac glucomannan composite porous particle, which comprises the following steps:
(1) preparing a suspension of baked fermented plant particles;
(2) adding a cross-linking agent into the suspension obtained in the step (1), and uniformly mixing to obtain a mixed solution;
(3) adding konjac glucomannan into the mixed solution obtained in the step (2), and mixing to obtain a gel mixture;
(4) reacting the gel-like mixture obtained in the step (3) at 50-120 ℃ for 2-8 h;
(5) freeze-drying the reaction product obtained in the step (4) until the dehydration is completed to form xerogel;
(6) and (3) crushing the dried gel obtained in the step (5), and screening the dried gel step by step to obtain particles with the particle size of 0.45mm-2mm, thus obtaining the baked fermented plant konjac glucomannan composite porous particles.
Preferably, the plant selected by the baked fermented plant particles is an aroma-containing plant, and the aroma-containing plant is one or a combination of dark plum, white snow tea, ciguatoside, pu' er tea, roxburgh rose, tobacco, black snow tea, sorghum, corn, coffee, tobacco leaf, dill seed, walnut shell, ganoderma lucidum, kudzu root, radix ophiopogonis, polished round-grained rice, glutinous rice, red rice, Chinese date, fennel, sarcandra glabra, rice, damnacanthus, Broussonetia papyrifera, radix isatidis, vinasse and the like; the preparation method of the baked fermented plant particles comprises the following steps:
firstly, sealing the dried plants at 120-200 ℃ and keeping for 2-8 hours for baking treatment;
secondly, spraying the product after baking treatment in the step I to bacillus subtilis Van3, and then fermenting for 24-72 hours at the temperature of 22 ℃ and the relative humidity of 60%;
and thirdly, crushing the product obtained after the fermentation in the step II into powder with the particle size of 100-180 meshes, and then bonding the powder into particles with the particle size of 20-60 meshes by using an adhesive, namely the baked fermented plant particles.
Preferably, the cross-linking agent in the step (2) is one or a combination of ammonia water, sodium hydroxide and sodium bicarbonate, and the amount of the cross-linking agent is 0.5-5.0 wt% of the water in the step (1); the addition amount of the konjac glucomannan in the step (3) is 1/50-1/10 of the water amount in the step (1), and the mass fraction of the konjac glucomannan in the baked fermented plant konjac glucomannan composite porous particles is not less than 2.8%.
Preferably, the freeze-drying temperature of step (4) is-20 ℃ to-50 ℃.
The third aspect of the invention discloses the application of the baked fermented plant konjac glucomannan composite porous particle in adsorption, harm removal and flavoring of tobacco filter sticks.
The invention has the beneficial effects that:
1. the structure of the composite porous particles of the roasted and fermented plant konjac glucomannan is that a three-dimensional network structure formed by KGM is used as a basic frame, the roasted and fermented plant particles are used as a filling material, and the crosslinking effect of KGM can wrap the roasted and fermented plant particles in the KGM to form the composite porous particles with higher porosity.
2. The preparation method of the composite porous particle of the roasted and fermented plant konjac glucomannan selects the roasted and fermented plant particle, and adjusts the mass ratio of the roasted and fermented plant particle to the konjac glucomannan, the dosage of deionized water, the type and dosage of an alkali cross-linking agent, the time and temperature of cross-linking reaction, the size of a product of the roasted and fermented plant particle, and the like, so that the prepared composite porous particle of the roasted and fermented plant konjac glucomannan shows better porosity and larger pore size.
3. The roasted and fermented plant konjac glucomannan composite porous particle has a porous structure, and the porous structure has certain through hole morphology characteristics; the specific surface area of the composite porous particles is 0.1523m in the particle diameter size range of 0.45mm-2mm2/g-7.5482m2The porosity is 10% -85%, and the pore size is 0.05-225 μm. Therefore, the baked fermented plant konjac glucomannan composite porous particle has higher porosity and pore size, and is an ideal porous structure material.
4. The baking fermented plant konjak glucomannan composite porous particle is used for adsorbing, removing harm and perfuming tobacco due to the characteristics of through holes and low suction resistance, and has the advantages of small adsorption resistance, stable and uniform volatilization of spices, good storage stability of cigarettes and lasting fragrance.
Drawings
Fig. 1 is an XRD spectrum of roasted fermented plant granules of corn sorghum black snow tea prepared in example 1 of the present invention.
Fig. 2 is an SEM electron microscope image of roasted fermented plant particles of corn sorghum black snow tea prepared in example 1 of the present invention, in which (a) is the overall morphology of the particles, and (b) is the surface pore structure of the specific single particles after enlargement; (c) to further enlarge the size of the rear surface pores.
Fig. 3 is a fourier infrared spectrum of baked fermented plant particles of corn sorghum black snow tea prepared in example 1 of the present invention.
FIG. 4 is the result of BET test on the baked fermented plant Konjac glucomannan composite porous particle prepared in example 1 of the present invention, wherein (a) is the isothermal N of the particle2Adsorption-desorption curves, (b) pore size distribution calculated by BJH method at the time of particle adsorption; (c) the pore size distribution calculated by BJH method during particle desorption;
FIG. 5 is SEM electron microscope appearance of the baked fermented plant konjac glucomannan composite porous particles prepared in the embodiment 1 of the invention; (a) the overall morphology of the composite porous particles, (b) the morphology of the local pore structure which is further enlarged; (c) new pores formed for the dehydration of KGM leading to surface damage;
Detailed Description
The following examples are a series of detailed descriptions of the preparation method and features of the present invention, and are not to be construed as limiting the claims of the present invention. It is also noted that several alternatives and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
Example 1
Preparing baked fermented plant particles of corn, sorghum and black snow tea:
putting the corn-sorghum black snow tea (wherein the weight parts are 4 parts of corn, 3 parts of sorghum and 1 part of black snow tea) into a carbonization furnace, gradually heating the furnace to about 80 ℃, keeping the temperature for 40min, quickly heating the temperature to 120 ℃ after the corn-sorghum black snow tea is dried, keeping the temperature for 3h, closing a heat source, and taking out a corn-sorghum black snow tea baking carbonization sample for later use (the weight of the corn-sorghum black snow tea is 50-80% of that before baking carbonization, and the common raw material is changed into grey brown).
② culture of Bacillus subtilis Van3 (B.subtiliss Van3)
A. Slant culture in test tubes
Luria-Bertani (LB) culture medium is adopted, and the formula is as follows: 10g of peptone, 10g of sodium chloride, 5g of yeast extract, 20g of agar and distilled water to reach the volume of 1000 ml. Sterilizing at 121 deg.C for 25 min, and placing on slant. Inoculating Van35, culturing at 28 deg.C for 24h to obtain test tube strain, transferring liquid strain into 1L LB liquid culture medium according to 5% (volume percentage of liquid strain, v/v), and shake culturing at 37 deg.C and 150r/min for 12 h; and centrifuging the culture solution at 3500r/min for 10min, washing the precipitate with sterile water, centrifuging, finally shaking the precipitate with 20mL of sterile water uniformly, and diluting the precipitate by 10 times when in use to obtain the bacillus subtilis Van 3.
B. Seed culture
Luria-Bertani (LB) culture medium is adopted, and the formula is as follows: 10g of peptone, 10g of sodium chloride, 5g of yeast extract and distilled water to reach the volume of 1000 ml. Sterilized at 121 ℃ for 25 minutes. Inoculating Van35 test tube strains, culturing at 28 ℃ for 24h to obtain liquid strains, transferring the liquid strains into 1L LB liquid culture medium according to the inoculum size of 5% (volume percentage of the liquid strains, v/v), and performing shake culture at 37 ℃ and 150r/min for 12 h; and centrifuging the culture solution at 3500r/min for 10min, washing the precipitate with sterile water, centrifuging, finally shaking the precipitate with 20mL of sterile water uniformly, and diluting the precipitate by 10 times when in use to obtain the bacillus subtilis Van 3.
③ fermentation of the roasted plants
Weighing 1000g of baked corn sorghum and black snow tea product, balancing the water content to 13 wt%, spraying 200mL of the obtained bacillus subtilis Van3, and then putting into a constant temperature and humidity box with the temperature of 22 ℃ and the relative humidity of 60% for fermentation for 48 h.
Preparation of baked fermented plant particles of corn, sorghum and black snow tea
Taking the fermentation sample, detecting the water content of the fermentation sample to be 10 wt%, and further crushing the fermentation sample into powder with the particle size of 120 meshes; then placing the powder into a Midi Glatt fluidized bed for granulation, and drying for 5min under the conditions that the fluidized air pressure of the fluidized bed is 0.2Bar and the airflow temperature is 60 ℃; then weighing 2 parts of gelatin and 8 parts of sodium carboxymethyl starch according to the parts by weight, and preparing a 10 wt% adhesive solution by using distilled water; applying 300g of the adhesive solution by adopting a top spraying mode under the conditions that the fluidizing air pressure is 0.25Bar, the air flow temperature is 60 ℃, the spraying pressure is 0.15Bar and the spraying speed is 12 g/min; after the adhesive is applied, drying for 5 minutes under the conditions that the fluidizing air pressure is 0.2Bar and the air flow temperature is 60 ℃ to prepare the baked fermented plant particles of the corn sorghum black snow tea, wherein the baked fermented plant particles have the moisture content of 12 wt%, the surface is rough and the particle size is 40 meshes.
The X-ray diffraction (XRD) pattern of the baked fermented plant granules of the prepared corn-sorghum-black snow tea is shown in figure 1. As can be seen from fig. 1: the diffraction peak on the XRD map is an amorphous diffraction broadening peak type with the peak position concentrated at 20 degrees, which indicates that the prepared baked fermented plant particles are in an amorphous phase, and the core component of the baked fermented plant particles can be determined to be amorphous carbon in consideration of the baking fermentation treatment process.
The SEM electron microscope appearance of the baked fermented plant particles of the prepared corn sorghum and black snow tea is shown in figure 2. As can be seen from fig. 2 (a): the particles are blocky as a whole and have no typical appearance, the particle size range is 0.68 mm-0.92 mm, and the average size is 0.64 +/-0.18 mm. Further enlarging to fig. 2(b), it can be seen that the surface is uneven, and there are some irregular deep holes (black depth of scene); the pore diameter measurement is shown in figure 2(c), and the result shows that the pore diameter of the smaller deep hole is concentrated about 30 μm, the pore distribution of the larger deep hole is wider, and the maximum pore diameter can reach 100.72 μm; the porosity was 34.52% as measured by the hanging weight method.
The Fourier infrared spectrum of the baked fermented plant granules of the prepared corn-sorghum-red snow tea is shown in figure 3. The main OH shown on the graph-Amide (NH)2N-H), aldehyde group (CH)2Infrared absorbing groups such as ═ CH-), olefin (C ═ C, C-H), acid anhydride (C ═ O, C-O-C), phosphoric acid group (P-O-C), and the presence of these groups indicates that the baking process is not complete, and there are residual plant-specific components in addition to the main phase amorphous carbon, and some of the specific components have efficacy of removing harmful components and enhancing flavor.
Preparing the baked fermented plant konjac glucomannan composite porous particles. The mass ratio of the konjac glucomannan is 12, and the mass ratio of the baked fermented plant particles is 63. The preparation steps are that (1) the dosage of solvent deionized water is 40 times of Konjac Glucomannan (KGM), and the baked fermented plant particles are dispersed into the deionized water to form suspension; adding an alkali cross-linking agent sodium hydroxide, and uniformly mixing, wherein the amount of the alkali cross-linking agent sodium hydroxide is 0.5 wt% of the amount of the deionized water; adding KGM, and continuously stirring until the KGM is converted into gel; step (4), performing crosslinking reaction on the gel-like mixture for 4 hours at the temperature of 105 ℃; step (5), placing the mixture at-35 ℃ for freeze drying and dehydration until the dehydration is complete to form xerogel; and (6) crushing the dried gel, and screening the dried gel step by step to obtain the baked fermented plant konjac glucomannan composite porous particles with the particle size range of 0.5-1 mm.
The prepared baked fermented plant konjac glucomannan composite porous particles are tested by a full-automatic specific surface and porosity analyzer, and the temperature is constant, N2The adsorption and desorption curves are shown in figure 4(a), and the pore size distribution of the composite porous particles under the adsorption and desorption conditions respectively calculated by BJH is shown in figure 4(b) and figure 4 (c). As can be seen from all the information of the BET test, the specific surface area of the composite porous particles was 0.5017m2(ii)/g, in the range of 1.7nm to 300nm, the cumulative surface area of the adsorption pores is 0.4451m2(iv)/g, cumulative surface area of desorption pores of 0.3183m2(ii) in terms of/g. The average pore diameter of the mesopores under adsorption and desorption is 8.3927nm and 10.8583nm, and the total surface area of the mesopores larger than 2nm is 0.196m2/g。
The shape of the prepared baked fermented plant konjac glucomannan composite porous particle is shown in figure 5. FIG. 5(a) shows the overall morphology of the composite porous particle with a transverse end dimension of about 1.28mm, which satisfies the particle size range after sieving. The konjac glucomannan is in a lamellar shape on the surface and has a characteristic wave or fold shape. At the position encircled in fig. 5(b), the thickness is significantly increased, potentially indicating that the roasted fermented plant particles are wrapped inside themselves by the swollen KGM when crosslinked. As shown by further enlarging fig. 5(b), the composite porous particle surface has distinct pores due to dehydration, and the pore size of the pores is poor, and the average size of the macropores is about 100 μm. As shown in fig. 5(c), it can be seen that the pore structure has pores formed by KGM surrounding each other, and some pores are formed by KGM self-breaking during dehydration.
Example 2
Preparation of baked fermented plant composite porous particles of white snow tea, ciguatoside and Pu' er tea is the same as example 1. The test results were similar to example 1.
Example 3
Preparation of baked fermented plant composite porous particles of polished round-grained rice, glutinous rice and red rice, the same as example 1. The test results were similar to example 1.
Example 4
The baked fermented plant konjac glucomannan composite porous particles prepared in the examples 1, 2 and 3 were added to a cigarette filter stick, and the baked fermented plant particles of the corn sorghum black snow tea of the example 1 were not compounded with konjac glucomannan as a comparison. The cigarettes of example 1, example 2 and example 3 and the control sample cigarettes were subjected to resistance-draw, whether the flavor was evenly volatilized, and storage stability tests, the results of which are shown in the following table:
TABLE 1 sample cigarette physical parameters
As can be seen from Table 1, the average quality and circumference of the sample cigarettes of the examples are consistent with those of the control cigarettes, and the cigarette smoking and testing requirements are met. The average smoking resistance of the cigarette added with the baked and fermented plant konjac glucomannan composite porous particles is lower than that of the particle cigarette without konjac glucomannan composite, and the smoking ease of the cigarette is improved to a certain extent.
TABLE 2 sensory evaluation scoring table
Compared with the control cigarette, the cigarette added with the baked fermented plant konjac glucomannan composite porous particles in the table 2 has the sensory evaluation score which is improved by 1.2 minutes compared with the average value of the control cigarette and is improved by 0.9 minute compared with the cigarette added with the porous particles which are not compounded with konjac glucomannan, mainly the richness and the fineness of the cigarette flavor are obviously improved, the whole style of the cigarette is kept unchanged, meanwhile, the fragrance is richer, the smoke concentration is improved, the irritation is reduced, the aftertaste is improved, and the smoking comfort is improved.
The cigarette is placed for 7 days and 30 days and then subjected to sensory evaluation, and the evaluation is carried out in a preposed constant temperature and humidity box and is balanced for 48 hours under the standard air humidity condition (the temperature is 22 +/-1 ℃, and the air humidity is 60 +/-1%). The cigarettes meeting the requirements are selected according to the industry standard YC/T138-1998 for sensory evaluation, and the results are shown in Table 3.
TABLE 3 sensory evaluation results
As can be seen from table 3 above, the cigarette added with the baked fermented plant konjac glucomannan composite porous particles has better aroma protection effect than the cigarette without the konjac glucomannan composite porous particles, so that the aroma has better stability and release uniformity, and better storage stability.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (10)
1. The composite porous particle is characterized by comprising konjac glucomannan and baked fermented plant particles, wherein the mass fraction of the baked fermented plant particles is 66.7-97.2, and the mass fraction of the konjac glucomannan is 2.8-33.3.
2. The baked fermented plant konjac glucomannan composite porous particle as claimed in claim 1, wherein the baked fermented plant particle is prepared by the following steps:
firstly, sealing the dried plants at 120-200 ℃ and keeping for 2-8 hours for baking treatment;
secondly, spraying the product after baking treatment in the step I to bacillus subtilis Van3, and then fermenting for 24-72 hours at the temperature of 22 ℃ and the relative humidity of 60%;
and thirdly, crushing the product obtained after the fermentation in the step II into powder with the particle size of 100-180 meshes, and then bonding the powder into particles with the particle size of 20-60 meshes by using an adhesive, namely the baked fermented plant particles.
3. The baked fermented plant konjac glucomannan composite porous particle according to claim 2, wherein the plant is a scented plant, and the scented plant is one or a combination of dark plum, white snow tea, ciguatin, pu' er tea, roxburgh rose, dry tobacco, red snow tea, sorghum, corn, coffee, tobacco leaf, dill seed, walnut shell, ganoderma lucidum, kudzu root, dwarf lilyturf tuber, polished round-grained rice, glutinous rice, red rice, Chinese date, fennel, sarcandra glabra, rice, jatropha, papermulberry orange peel, radix isatidis, vinasse and the like.
4. The baked fermented plant konjac glucomannan composite porous particle according to claim 1, wherein the baked fermented plant konjac glucomannan composite porous particle is a porous structure; the baked fermented plant konjac glucomannan composite porous particle takes a three-dimensional network formed by the konjac glucomannan as a frame, takes the baked fermented plant particle as a filling material, and is wrapped in the konjac glucomannan.
5. The baked fermented plant konjac glucomannan composite porous particle according to claim 1, wherein the baked fermented plant konjac glucomannan composite porous particle has a diameter of 0.45mm to 2mm, a porosity of 10% to 85%, and a pore size of 0.05 μm to 225 μm; the specific surface area is 0.1523m2/g-7.5482m2/g。
6. A preparation method of a baking fermented plant konjac glucomannan composite porous particle is characterized by comprising the following steps:
(1) preparing a suspension of baked fermented plant particles;
(2) adding a cross-linking agent into the suspension obtained in the step (1), and uniformly mixing to obtain a mixed solution;
(3) adding konjac glucomannan into the mixed solution obtained in the step (2), and mixing to obtain a gel mixture;
(4) reacting the gel-like mixture obtained in the step (3) at 50-120 ℃ for 2-8 h;
(5) freeze-drying the reaction product obtained in the step (4) until the dehydration is completed to form xerogel;
(6) and (3) crushing the dried gel obtained in the step (5), and screening the dried gel step by step to obtain particles with the particle size of 0.45mm-2mm, thus obtaining the baked fermented plant konjac glucomannan composite porous particles.
7. The preparation method according to claim 6, wherein the plant selected from the baked fermented plant particles is an aroma-containing plant, and the aroma-containing plant is one or a combination of dark plum, white snow tea, ciguatin, pu' er tea, roxburgh rose, dry tobacco, red snow tea, sorghum, corn, coffee, tobacco leaf, dill seed, walnut shell, ganoderma lucidum, kudzu root, dwarf lilyturf tuber, polished round-grained rice, glutinous rice, red rice, jujube, fennel, sarcandra glabra, rice, elsholtzia, Broussonetia papyrifera flava, radix isatidis, vinasse and the like; the preparation method of the baked fermented plant particles comprises the following steps:
firstly, sealing the dried plants at 120-200 ℃ and keeping for 2-8 hours for baking treatment;
secondly, spraying the product after baking treatment in the step I to bacillus subtilis Van3, and then fermenting for 24-72 hours at the temperature of 22 ℃ and the relative humidity of 60%;
and thirdly, crushing the product obtained after the fermentation in the step II into powder with the particle size of 100-180 meshes, and then bonding the powder into particles with the particle size of 20-60 meshes by using an adhesive, namely the baked fermented plant particles.
8. The preparation method according to claim 6, wherein the cross-linking agent in step (2) is one or a combination of ammonia water, sodium hydroxide and sodium bicarbonate, and the amount of the cross-linking agent is 0.5-5.0 wt% of the water in step (1); the addition amount of the konjac glucomannan in the step (3) is 1/50-1/10 of the water amount in the step (1), and the mass fraction of the konjac glucomannan in the baked fermented plant konjac glucomannan composite porous particles is not less than 2.8%.
9. The process according to claim 6, wherein the freeze-drying temperature in the step (4) is from-20 ℃ to-50 ℃.
10. The use of the roasted and fermented plant konjac glucomannan composite porous particles according to any one of claims 1 to 5 for adsorbing, detoxifying and perfuming in tobacco filter sticks.
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Application publication date: 20210430 |