CN107513891B - Dried orange peel cigarette paper with moisture retention function and preparation method thereof - Google Patents
Dried orange peel cigarette paper with moisture retention function and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
- D21H21/52—Additives of definite length or shape
- D21H21/54—Additives of definite length or shape being spherical, e.g. microcapsules, beads
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/02—Material of vegetable origin
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/64—Alkaline compounds
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The invention discloses dried orange peel cigarette paper with a moisturizing function and a preparation method of the dried orange peel cigarette paper. The hydroxyapatite hollow microspheres loaded with the spices are used as the cigarette paper additive to prepare the dried orange peel cigarette paper with the moisture retention function, and the dried orange peel cigarette paper has the characteristics of good treatment effect, low cost, easiness in operation and the like.
Description
Technical Field
The invention belongs to the technical field of cigarette processing, and particularly relates to dried orange peel cigarette paper with a moisture retention function and a preparation method thereof.
Background
Along with the promotion of tar and harm reduction work in the tobacco industry, the tar content of cigarettes is gradually reduced, and accordingly, the aroma amount of the cigarettes is insufficient, and the dry feeling is enhanced. In order to improve the sensory quality of cigarettes, the tobacco industry carries out research on aroma enhancement and moisture retention as one of nine major items of the compendium of long-term scientific and technological development in the tobacco industry while reducing tar and harm. At present, the research on cigarette flavoring and moisture retention mainly focuses on tobacco shreds or filter tips, and is embodied in the aspects of development of novel flavor raw materials and research on a moisture retention agent, namely, the flavor raw materials with the functions of flavoring and moisture retention are added on the tobacco shreds or the tobacco bundles, and the research on the cigarette paper with the functions of flavoring and moisture retention is less. Such as: anrui et al (anrui, xie yi min, wangyi, royal phoenix, yaoyuan army, preparation and performance research of tobacco sheet type cigarette paper, china paper making, 2012, 31 (1): 45-48) coated the tobacco stem extract on the cigarette paper, scholars (huangfu, liu, wangyun, development and application of characteristic mint type cigarette paper, china paper making, 2012, 31 (1): 42-44) coated natural plants such as mint extract on the cigarette paper.
The cigarette paper is a special thin-leaf paper for wrapping tobacco to make cigarettes. Compared with other cigarette auxiliary materials such as tipping paper and forming paper, the cigarette additive mainly participates in combustion, so that unfavorable wood gas is generated for smoke of the cigarette in the combustion process of the cigarette, and the adjustment and improvement of the performance of the cigarette paper through the cigarette paper additive are particularly important. In addition, the cigarette paper can also be used as an attachment of spice, and a feasible way is to add the spice on the cigarette paper to strengthen the product characteristics.
However, through research, the researchers find that most of the extracted effective components are organic matters and have the characteristic of volatility, and the extracted effective components are added to cigarette paper or tobacco sheets in a coating mode to easily generate serious consequences that the fragrance loss is serious or the fragrance loss is difficult to last, and the burning speed, the ventilation degree, the suction opening number and the main (side) flow smoke of the cigarette are difficult to control. The patent adopts a new technology to load the fragrant substances on the surface of the hollow hydroxyapatite, so that the added aroma-enhancing organic matters can keep the fragrance for a long time, and the cigarettes are endowed with different functional feelings and senses. The surface of the hollow hydroxyapatite is of a porous structure, the interior of the hollow hydroxyapatite is of a hollow structure, and the special structure enables the hollow hydroxyapatite to have the advantages of light specific gravity, large adsorption capacity, high load efficiency and the like. Meanwhile, the hollow hydroxyapatite is widely applied to the medical fields of tissue repair and the like and has no toxicity.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide the dried orange peel cigarette paper with the moisture retention function, and the dried orange peel cigarette paper has certain functions of increasing aroma and retaining moisture.
The invention also provides a preparation method of the dried orange peel cigarette paper with the moisture retention function.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) stirring and dispersing spherical calcium carbonate in a disodium hydrogen phosphate solution, adjusting the pH value to 10-12, carrying out hydrothermal reaction at 110-130 ℃ for 0.5-1.5 hours, cooling to room temperature, carrying out solid-liquid separation, taking the solid, and drying to obtain hydroxyapatite hollow microspheres; wherein the mass ratio of the spherical calcium carbonate to the disodium hydrogen phosphate is 1: 0.04 to 0.06;
(2) adding the hydroxyapatite hollow microspheres obtained in the step (1) and perfume into water, stirring for 40-55 hours, carrying out solid-liquid separation, washing and drying solids to obtain perfume-loaded hydroxyapatite hollow microspheres; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1-0.3, and mixing;
(3) spraying the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (2) on cigarette paper to obtain the dried orange peel cigarette paper; or adding the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (2) into paper pulp, and then preparing the dried orange peel cigarette paper.
Preferably, the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 10-30% of the weight of the dried orange peel cigarette paper.
Preferably, the spherical calcium carbonate in step (1) is prepared according to the following steps: adding a sodium carbonate solution into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate, stirring for 0.5-2 hours, carrying out solid-liquid separation, washing and drying solids to obtain the sodium polystyrene sulfonate-containing sodium carbonate solid-liquid composite material; wherein the mol ratio of the sodium carbonate to the calcium chloride to the sodium polystyrene sulfonate is 1: 0.9-1.1: 0.9 to 1.1.
Preferably, the concentration of the disodium hydrogen phosphate solution in the step (1) is 0.08-0.12 g/L.
Preferably, the dried orange peel extract in the step (2) is prepared according to the following steps: cleaning pericarpium Citri Tangerinae, sterilizing, pulverizing, adding mixed solution of water and ethanol, reflux-extracting at 55-65 deg.C for 2.5-3.5 hr, performing solid-liquid separation to obtain filtrate, and freeze-drying to obtain the final product; wherein the mixed solution of water and ethanol is prepared from water and ethanol according to the volume ratio of 1: 0.5-1.5 and uniformly mixing.
Preferably, the mass ratio of the hydroxyapatite hollow microspheres to the perfume in the step (2) is 10: 0.01 to 1.
The dried orange peel cigarette paper with the moisture retention function is prepared by the method.
According to the invention, the cigarette paper is added with the hydroxyapatite hollow microsphere material loaded with the spice to prepare the dried orange peel cigarette paper with the moisture retention function, and the hydroxyapatite hollow microsphere loaded with the spice is used as a cigarette paper additive, so that the cigarette can be endowed with a certain dried orange peel taste and cool taste, and positive effects on improving the cigarette taste and reducing the cigarette irritation are achieved.
Drawings
FIG. 1 is a graph showing the moisture retention performance test of the sample cigarette and the blank cigarette described in example 1.
Detailed Description
In order to make the technical purpose, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are further described with reference to specific examples, which are intended to explain the present invention and are not to be construed as limiting the present invention, and those who do not specify a specific technique or condition in the examples follow the techniques or conditions described in the literature in the art or follow the product specification. The preparation of the cigarette paper in the following examples can be realized by adopting the conventional process in the prior art, which is not innovative in the invention and is not described in detail.
Sodium polystyrene sulfonate (PSS) described in the examples below was purchased from Shanghai Biotech Inc. (CAS: 25704-18-1). The menthol (CAS: 89-78-1) was purchased from Guangzhou daily chemical Co., Ltd.
The dried orange peel extract of the following examples 1 and 2 was prepared according to the following procedure: cleaning pericarpium Citri Tangerinae, sterilizing, pulverizing, adding mixed solution of water and ethanol (water and ethanol are mixed at volume ratio of 1: 1), reflux extracting at 60 deg.C for 3 hr, filtering, collecting filtrate, adding the same amount of mixed solution of water and ethanol into the residue, reflux extracting at 60 deg.C for 1 hr, filtering to remove filtrate, mixing the filtrates, centrifuging at high speed to remove impurities, and freeze drying the supernatant.
The dried orange peel extract of the following examples 3 and 4 was prepared according to the following procedure: cleaning pericarpium Citri Tangerinae, sterilizing, pulverizing, adding mixed solution of water and ethanol (water and ethanol are mixed at volume ratio of 1: 0.5), reflux-extracting at 65 deg.C for 2.5 hr, filtering, collecting filtrate, adding the same amount of mixed solution of water and ethanol into the residue, reflux-extracting at 65 deg.C for 1 hr, filtering to remove filtrate, mixing the filtrates, centrifuging by high speed centrifuge to remove impurities, and freeze-drying the supernatant.
The following dried orange peel extracts of examples 5 and 6 were prepared according to the following procedure: cleaning pericarpium Citri Tangerinae, sterilizing, pulverizing, adding mixed solution of water and ethanol (water and ethanol are mixed at volume ratio of 1: 1.5), reflux-extracting at 55 deg.C for 3.5 hr, filtering, collecting filtrate, adding the same amount of mixed solution of water and ethanol into the residue, reflux-extracting at 55 deg.C for 1 hr, filtering to remove filtrate, mixing the filtrates, centrifuging at high speed to remove impurities, and freeze-drying the supernatant.
Example 1
A preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) under the condition of room temperature, quickly adding 10 mL of calcium chloride solution with the concentration of 0.5 mol/L into 100 mL of sodium polystyrene sulfonate solution with the concentration of 10 mg/mL, and uniformly stirring and mixing by magnetic force to obtain an aqueous solution containing calcium chloride and sodium polystyrene sulfonate; under the stirring condition, 10 mL of sodium carbonate solution with the concentration of 0.5 mol/L is dropwise added into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate at the speed of 1 mL/min by using a constant flow pump to generate white precipitates, after the dropwise addition of the sodium carbonate solution is finished, the mixture is stirred for 1 hour, then the mixture is centrifugally separated by an ultracentrifuge (8000 rpm,3 minutes) to obtain precipitates, the precipitates are respectively washed for 3 times by deionized water and absolute ethyl alcohol, and the precipitates are dried for 24 hours at the temperature of 60 ℃ to obtain spherical calcium carbonate;
(2) placing 0.2 g of the spherical calcium carbonate obtained in the step (1) in a beaker, quickly adding 100 mL of 0.1 g/L disodium hydrogen phosphate solution into the beaker, and stirring by magnetic force to obtain a suspension; adjusting the pH value of the suspension to 11 by using 1 mol/L NaOH solution, transferring the suspension in the beaker to a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 1 hour at 120 ℃, taking out the suspension after the reaction is finished, cooling the suspension, carrying out centrifugal separation (8000 rpm,3 min), washing the solid with deionized water and absolute ethyl alcohol for 3 times respectively, and drying the solid for 24 hours at 60 ℃ to obtain hydroxyapatite hollow microspheres;
(3) adding 100 mg of the hydroxyapatite hollow microsphere obtained in the step (2) and 10 mg of perfume into 10 mL of water, stirring for 48 hours, carrying out solid-liquid separation, washing and drying the solid to obtain a perfume-loaded hydroxyapatite hollow microsphere; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1, mixing evenly;
(4) spraying the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (3) on cigarette paper to obtain the dried orange peel cigarette paper; the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 10% of the weight of the cigarette paper with the dried orange peel.
The dried orange peel cigarette paper with the moisture retention function is prepared by the method.
And respectively rolling cigarette samples by using the prepared tangerine peel cigarette paper and common cigarette paper with the same quantitative air permeability by using the same tobacco shreds, and respectively marking as a sample cigarette and a blank cigarette. The prepared sample cigarette and blank cigarette are placed in an environment with the temperature of 22 +/-1 ℃ and the relative humidity of 60 +/-2% for balancing 48h, then the sample cigarette and the blank cigarette are placed in an environment with the temperature of 22 +/-1 ℃ and the relative humidity of 40 +/-2% for inspecting the moisture-removing process, and the change of the instant moisture content is analyzed, and the result is shown in figure 1.
As can be seen from figure 1, compared with a blank cigarette, the moisture loss rate of the sample cigarette is slower, because hydroxyl contained in the hydroxyapatite hollow microspheres can form hydrogen bonds with water to bind the water, the moisture loss is delayed, and the physical moisture retention performance of the tobacco shreds is improved.
The prepared cigarette paper containing the dried orange peel and the common cigarette paper with the same quantitative air permeability are respectively rolled into cigarette samples by adopting the same tobacco shreds, the cigarette samples are respectively marked as a sample cigarette and a blank cigarette, the blank cigarette is taken as a comparative example, and the method is carried out according to the fourth part of the cigarette of GB 5606.4-2005: sensory technical requirements the sensory quality of the cigarettes was evaluated according to the criteria of the sensory standards, and the results are shown in table 1.
TABLE 1 cigarette sensory quality evaluation
As can be seen from the table 1, when the cigarette paper containing the dried orange peel is used in cigarettes, the fragrance score of the cigarettes is increased compared with that of a comparison sample, the cigarettes have cool flavor and dried orange peel fragrance, other indexes are basically unchanged, and the sensory quality is improved totally.
Example 2
A preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) under the condition of room temperature, quickly adding 10 mL of calcium chloride solution with the concentration of 0.5 mol/L into 100 mL of sodium polystyrene sulfonate solution with the concentration of 10 mg/mL, and uniformly stirring and mixing by magnetic force to obtain an aqueous solution containing calcium chloride and sodium polystyrene sulfonate; under the stirring condition, 10 mL of sodium carbonate solution with the concentration of 0.5 mol/L is dropwise added into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate at the speed of 1 mL/min by using a constant flow pump to generate white precipitates, after the dropwise addition of the sodium carbonate solution is finished, the mixture is stirred for 0.5 hour, then the mixture is centrifugally separated by an ultracentrifuge (8000 rpm,3 min) to obtain precipitates, the precipitates are respectively washed for 3 times by deionized water and absolute ethyl alcohol, and the precipitates are dried for 24 hours at the temperature of 60 ℃ to obtain spherical calcium carbonate;
(2) placing 0.2 g of the spherical calcium carbonate obtained in the step (1) in a beaker, quickly adding 100 mL of 0.08 g/L disodium hydrogen phosphate solution into the beaker, and stirring by magnetic force to obtain a suspension; adjusting the pH value of the suspension to 12 by using 1 mol/L NaOH solution, transferring the suspension in the beaker to a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 1.5 hours at 110 ℃, taking out the suspension after the reaction is finished, cooling the suspension, carrying out centrifugal separation (8000 rpm,3 min), washing the solid with deionized water and absolute ethyl alcohol for 3 times respectively, and drying the solid for 24 hours at 60 ℃ to obtain hydroxyapatite hollow microspheres;
(3) adding 100 mg of the hydroxyapatite hollow microsphere obtained in the step (2) and 0.1 mg of spice into 10 mL of water, stirring for 40 hours, carrying out solid-liquid separation, washing and drying the solid to obtain a spice-loaded hydroxyapatite hollow microsphere; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1, mixing evenly;
(4) spraying the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (3) on cigarette paper to obtain the dried orange peel cigarette paper; the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 30% of the weight of the dried orange peel cigarette paper.
Example 3
A preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) under the condition of room temperature, quickly adding 10 mL of calcium chloride solution with the concentration of 0.5 mol/L into 100 mL of sodium polystyrene sulfonate solution with the concentration of 10 mg/mL, and uniformly stirring and mixing by magnetic force to obtain an aqueous solution containing calcium chloride and sodium polystyrene sulfonate; under the stirring condition, 10 mL of sodium carbonate solution with the concentration of 0.5 mol/L is dropwise added into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate at the speed of 1 mL/min by using a constant flow pump to generate white precipitates, after the dropwise addition of the sodium carbonate solution is finished, the mixture is stirred for 1.5 hours, then the mixture is centrifugally separated by an ultracentrifuge (8000 rpm,3 minutes) to obtain precipitates, the precipitates are respectively washed for 3 times by deionized water and absolute ethyl alcohol, and the precipitates are dried for 24 hours at the temperature of 60 ℃ to obtain spherical calcium carbonate;
(2) placing 0.2 g of the spherical calcium carbonate obtained in the step (1) in a beaker, quickly adding 100 mL of 0.12 mg/L disodium hydrogen phosphate solution into the beaker, and stirring by magnetic force to obtain a suspension; adjusting the pH value of the suspension to 10 by using 1 mol/L NaOH solution, transferring the suspension in the beaker to a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 0.5 hour at 130 ℃, taking out the suspension after the reaction is finished, cooling the suspension, carrying out centrifugal separation (8000 rpm,3 min), washing the solid with deionized water and absolute ethyl alcohol for 3 times respectively, and drying the solid for 24 hours at 60 ℃ to obtain hydroxyapatite hollow microspheres;
(3) adding 100 mg of the hydroxyapatite hollow microsphere obtained in the step (2) and 1 mg of spice into 10 mL of water, stirring for 50 hours, carrying out solid-liquid separation, washing and drying the solid to obtain a spice-loaded hydroxyapatite hollow microsphere; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.2, mixing evenly;
(4) spraying the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (3) on cigarette paper to obtain the dried orange peel cigarette paper; the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 20% of the weight of the cigarette paper with the dried orange peel.
Example 4
A preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) under the condition of room temperature, quickly adding 10 mL of calcium chloride solution with the concentration of 0.5 mol/L into 100 mL of sodium polystyrene sulfonate solution with the concentration of 10 mg/mL, and uniformly stirring and mixing by magnetic force to obtain an aqueous solution containing calcium chloride and sodium polystyrene sulfonate; under the stirring condition, 10 mL of sodium carbonate solution with the concentration of 0.5 mol/L is dropwise added into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate at the speed of 1 mL/min by using a constant flow pump to generate white precipitates, after the dropwise addition of the sodium carbonate solution is finished, the mixture is stirred for 1 hour, then the mixture is centrifugally separated by an ultracentrifuge (8000 rpm,3 minutes) to obtain precipitates, the precipitates are respectively washed for 3 times by deionized water and absolute ethyl alcohol, and the precipitates are dried for 24 hours at the temperature of 60 ℃ to obtain spherical calcium carbonate;
(2) placing 0.2 g of the spherical calcium carbonate obtained in the step (1) in a beaker, quickly adding 100 mL of 0.1 g/L disodium hydrogen phosphate solution into the beaker, and stirring by magnetic force to obtain a suspension; adjusting the pH value of the suspension to 11 by using 1 mol/L NaOH solution, transferring the suspension in the beaker to a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 1 hour at 120 ℃, taking out the suspension after the reaction is finished, cooling the suspension, carrying out centrifugal separation (8000 rpm,3 min), washing the solid with deionized water and absolute ethyl alcohol for 3 times respectively, and drying the solid for 24 hours at 60 ℃ to obtain hydroxyapatite hollow microspheres;
(3) adding 100 mg of the hydroxyapatite hollow microsphere obtained in the step (2) and 10 mg of perfume into 10 mL of water, stirring for 48 hours, carrying out solid-liquid separation, washing and drying the solid to obtain a perfume-loaded hydroxyapatite hollow microsphere; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.3, mixing evenly;
(4) adding the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (3) into paper pulp, and then preparing the dried orange peel cigarette paper; the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 10% of the weight of the cigarette paper with the dried orange peel.
Example 5
A preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) under the condition of room temperature, quickly adding 10 mL of calcium chloride solution with the concentration of 0.5 mol/L into 100 mL of sodium polystyrene sulfonate solution with the concentration of 10 mg/mL, and uniformly stirring and mixing by magnetic force to obtain an aqueous solution containing calcium chloride and sodium polystyrene sulfonate; under the stirring condition, 10 mL of sodium carbonate solution with the concentration of 0.5 mol/L is dropwise added into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate at the speed of 1 mL/min by using a constant flow pump to generate white precipitates, after the dropwise addition of the sodium carbonate solution is finished, the mixture is stirred for 0.5 hour, then the mixture is centrifugally separated by an ultracentrifuge (8000 rpm,3 min) to obtain precipitates, the precipitates are respectively washed for 3 times by deionized water and absolute ethyl alcohol, and the precipitates are dried for 24 hours at the temperature of 60 ℃ to obtain spherical calcium carbonate;
(2) placing 0.2 g of the spherical calcium carbonate obtained in the step (1) in a beaker, quickly adding 100 mL of 0.08 g/L disodium hydrogen phosphate solution into the beaker, and stirring by magnetic force to obtain a suspension; adjusting the pH value of the suspension to 12 by using 1 mol/L NaOH solution, transferring the suspension in the beaker to a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 1.5 hours at 110 ℃, taking out the suspension after the reaction is finished, cooling the suspension, carrying out centrifugal separation (8000 rpm,3 min), washing the solid with deionized water and absolute ethyl alcohol for 3 times respectively, and drying the solid for 24 hours at 60 ℃ to obtain hydroxyapatite hollow microspheres;
(3) adding 100 mg of the hydroxyapatite hollow microsphere obtained in the step (2) and 0.1 mg of spice into 10 mL of water, stirring for 40 hours, carrying out solid-liquid separation, washing and drying the solid to obtain a spice-loaded hydroxyapatite hollow microsphere; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.3, mixing evenly;
(4) adding the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (3) into paper pulp, and then preparing the dried orange peel cigarette paper; the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 30% of the weight of the dried orange peel cigarette paper.
Example 6
A preparation method of the dried orange peel cigarette paper with the moisture retention function comprises the following steps:
(1) under the condition of room temperature, quickly adding 10 mL of calcium chloride solution with the concentration of 0.5 mol/L into 100 mL of sodium polystyrene sulfonate solution with the concentration of 10 mg/mL, and uniformly stirring and mixing by magnetic force to obtain an aqueous solution containing calcium chloride and sodium polystyrene sulfonate; under the stirring condition, 10 mL of sodium carbonate solution with the concentration of 0.5 mol/L is dropwise added into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate at the speed of 1 mL/min by using a constant flow pump to generate white precipitates, after the dropwise addition of the sodium carbonate solution is finished, the mixture is stirred for 1.5 hours, then the mixture is centrifugally separated by an ultracentrifuge (8000 rpm,3 minutes) to obtain precipitates, the precipitates are respectively washed for 3 times by deionized water and absolute ethyl alcohol, and the precipitates are dried for 24 hours at the temperature of 60 ℃ to obtain spherical calcium carbonate;
(2) placing 0.2 g of the spherical calcium carbonate obtained in the step (1) in a beaker, quickly adding 100 mL of 0.12 mg/L disodium hydrogen phosphate solution into the beaker, and stirring by magnetic force to obtain a suspension; adjusting the pH value of the suspension to 10 by using 1 mol/L NaOH solution, transferring the suspension in the beaker to a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction for 0.5 hour at 130 ℃, taking out the suspension after the reaction is finished, cooling the suspension, carrying out centrifugal separation (8000 rpm,3 min), washing the solid with deionized water and absolute ethyl alcohol for 3 times respectively, and drying the solid for 24 hours at 60 ℃ to obtain hydroxyapatite hollow microspheres;
(3) adding 100 mg of the hydroxyapatite hollow microsphere obtained in the step (2) and 1 mg of spice into 10 mL of water, stirring for 55 hours, carrying out solid-liquid separation, washing and drying the solid to obtain a spice-loaded hydroxyapatite hollow microsphere; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.2, mixing evenly;
(4) adding the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (3) into paper pulp, and then preparing the dried orange peel cigarette paper; the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 20% of the weight of the cigarette paper with the dried orange peel.
The dried orange peel cigarette paper with the moisture retention function prepared by the methods in the embodiments 2-6 has cool taste and dried orange peel fragrance, is overall improved in sensory quality, and has the moisture retention effect equivalent to that in the embodiment 1.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The dried orange peel cigarette paper with the moisture retention function is characterized by being prepared by the following steps:
(1) stirring and dispersing spherical calcium carbonate in a disodium hydrogen phosphate solution, adjusting the pH value to 10-12, carrying out hydrothermal reaction at 110-130 ℃ for 0.5-1.5 hours, cooling to room temperature, carrying out solid-liquid separation, taking the solid, and drying to obtain hydroxyapatite hollow microspheres; wherein the mass ratio of the spherical calcium carbonate to the disodium hydrogen phosphate is 1: 0.04 to 0.06;
(2) mixing the hydroxyapatite hollow microspheres obtained in the step (1) and an aroma according to a mass ratio of 10: 0.01-1, adding the mixture into water, stirring for 40-55 hours, carrying out solid-liquid separation, washing and drying solids to obtain the hydroxyapatite hollow microspheres loaded with the perfume; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1-0.3, and mixing;
the dried orange peel extract is prepared according to the following steps: cleaning pericarpium Citri Tangerinae, sterilizing, pulverizing, adding mixed solution of water and ethanol, reflux-extracting at 55-65 deg.C for 2.5-3.5 hr, performing solid-liquid separation to obtain filtrate, and freeze-drying to obtain the final product; wherein the mixed solution of water and ethanol is prepared from water and ethanol according to the volume ratio of 1: 0.5-1.5, and uniformly mixing;
(3) spraying the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (2) on cigarette paper to obtain the dried orange peel cigarette paper; or adding the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (2) into paper pulp, and then preparing the dried orange peel cigarette paper.
2. The dried orange peel cigarette paper with the moisture retention function according to claim 1, characterized in that: the pH value in the step (1) is 11; the mass ratio of the spherical calcium carbonate to the disodium hydrogen phosphate is 1: 0.05;
in the step (2), the mass ratio of the hydroxyapatite hollow microspheres to the perfume is 10: 1; the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1 or 1: 0.3, mixing evenly;
the addition amount of the hydroxyapatite hollow microspheres loaded with the spices in the step (3) accounts for 10% of the weight of the dried orange peel cigarette paper.
3. The dried orange peel cigarette paper with the moisture retention function according to claim 1, characterized in that: the pH value in the step (1) is 10; the mass ratio of the spherical calcium carbonate to the disodium hydrogen phosphate is 1: 0.06;
in the step (2), the mass ratio of the hydroxyapatite hollow microspheres to the perfume is 10: 0.1; the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.2, mixing evenly;
the addition amount of the hydroxyapatite hollow microspheres loaded with the spices in the step (3) accounts for 20% of the weight of the dried orange peel cigarette paper.
4. The dried orange peel cigarette paper with the moisture retention function according to claim 1, characterized in that: the pH value in the step (1) is 12; the mass ratio of the spherical calcium carbonate to the disodium hydrogen phosphate is 1: 0.04;
in the step (2), the mass ratio of the hydroxyapatite hollow microspheres to the perfume is 10: 0.01; the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1 or 1: 0.3, mixing evenly;
the addition amount of the hydroxyapatite hollow microspheres loaded with the spices in the step (3) accounts for 30% of the weight of the dried orange peel cigarette paper.
5. The preparation method of the dried orange peel cigarette paper with the moisture retention function as claimed in claim 1, is characterized by comprising the following steps:
(1) stirring and dispersing spherical calcium carbonate in a disodium hydrogen phosphate solution, adjusting the pH value to 10-12, carrying out hydrothermal reaction at 110-130 ℃ for 0.5-1.5 hours, cooling to room temperature, carrying out solid-liquid separation, taking the solid, and drying to obtain hydroxyapatite hollow microspheres; wherein the mass ratio of the spherical calcium carbonate to the disodium hydrogen phosphate is 1: 0.04 to 0.06;
(2) mixing the hydroxyapatite hollow microspheres obtained in the step (1) and an aroma according to a mass ratio of 10: 0.01-1, adding the mixture into water, stirring for 40-55 hours, carrying out solid-liquid separation, washing and drying solids to obtain the hydroxyapatite hollow microspheres loaded with the perfume; wherein the spice is prepared from dried orange peel extract and menthol according to a mass ratio of 1: 0.1-0.3, and mixing;
the dried orange peel extract is prepared according to the following steps: cleaning pericarpium Citri Tangerinae, sterilizing, pulverizing, adding mixed solution of water and ethanol, reflux-extracting at 55-65 deg.C for 2.5-3.5 hr, performing solid-liquid separation to obtain filtrate, and freeze-drying to obtain the final product; wherein the mixed solution of water and ethanol is prepared from water and ethanol according to the volume ratio of 1: 0.5-1.5, and uniformly mixing;
(3) spraying the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (2) on cigarette paper to obtain the dried orange peel cigarette paper; or adding the hydroxyapatite hollow microspheres loaded with the spices obtained in the step (2) into paper pulp, and then preparing the dried orange peel cigarette paper.
6. The preparation method of the dried orange peel cigarette paper with the moisture retention function according to claim 5, which is characterized in that: the addition amount of the hydroxyapatite hollow microspheres loaded with the spices accounts for 10-30% of the weight of the dried orange peel cigarette paper.
7. The preparation method of the dried orange peel cigarette paper with the moisture retention function according to claim 5, which is characterized in that: the concentration of the disodium hydrogen phosphate solution in the step (1) is 0.08-0.12 g/L.
8. The method for preparing the dried orange peel cigarette paper with the moisture retention function according to claim 5, wherein the spherical calcium carbonate in the step (1) is prepared according to the following steps: adding a sodium carbonate solution into an aqueous solution containing calcium chloride and sodium polystyrene sulfonate, stirring for 0.5-2 hours, carrying out solid-liquid separation, washing and drying solids to obtain the sodium polystyrene sulfonate-containing sodium carbonate solid-liquid composite material; wherein the mol ratio of the sodium carbonate to the calcium chloride to the sodium polystyrene sulfonate is 1: 0.9-1.1: 0.9 to 1.1.
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| CN108433169B (en) * | 2018-03-14 | 2020-11-17 | 河南中烟工业有限责任公司 | Method for storing cigarette tobacco rich in orange sweet fragrance |
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| DK2505615T3 (en) * | 2011-04-01 | 2014-08-04 | Omya Int Ag | Self-binding pigment hybrid |
| CN103711029B (en) * | 2013-12-20 | 2015-07-01 | 华南理工大学 | Method for manufacturing aroma-increasing moisture retention cigarette paper |
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