CN111789286A - Porous frame solid bead and preparation method and application thereof - Google Patents

Porous frame solid bead and preparation method and application thereof Download PDF

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Publication number
CN111789286A
CN111789286A CN202010503989.3A CN202010503989A CN111789286A CN 111789286 A CN111789286 A CN 111789286A CN 202010503989 A CN202010503989 A CN 202010503989A CN 111789286 A CN111789286 A CN 111789286A
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China
Prior art keywords
porous
porous frame
frame solid
bead
carboxymethyl cellulose
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Pending
Application number
CN202010503989.3A
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Chinese (zh)
Inventor
孙继勇
厉昌坤
于浩
王琦琦
孟宪良
王芳俊川
何思
王艳梅
马晓龙
张远方
周德彪
王胜堂
曹斐
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Shandong Jiangjun Tobacco New Material Technology Co ltd
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Shandong Jiangjun Tobacco New Material Technology Co ltd
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Priority to CN202010503989.3A priority Critical patent/CN111789286A/en
Publication of CN111789286A publication Critical patent/CN111789286A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/04Tobacco smoke filters characterised by their shape or structure
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/08Use of materials for tobacco smoke filters of organic materials as carrier or major constituent
    • A24D3/10Use of materials for tobacco smoke filters of organic materials as carrier or major constituent of cellulose or cellulose derivatives

Abstract

The invention relates to a porous frame solid bead and a preparation method and application thereof. The solid bead is in a porous net structure, porous channels are formed in the solid bead, and the carboxymethyl cellulose, the adsorbing material and the cooling material are composed of, by weight, 30-50 parts of carboxymethyl cellulose, 10-30 parts of the adsorbing material and 20-40 parts of the cooling material. Also comprises a fragrance slow-release material. The adsorbing material is graphene or diatomite. The cooling material is pottery clay or silica gel. The porous frame solid beads have the advantages of long adsorption time and good filtering, cooling and aroma-enhancing effects.

Description

Porous frame solid bead and preparation method and application thereof
Technical Field
The invention belongs to the technical field of cigarette filter sticks, and particularly relates to a porous frame solid bead and a preparation method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The conventional filter stick of the cigarette is added with the popping beads, so that the smoke is flavored, and the experience degree is improved. With the development of the technology, the flavor is added separately, and a series of uncomfortable feelings such as dryness generated by smoke generated by cigarettes cannot be solved. As smoke passes through the filter stick, the temperature of the filter stick is high, and the filter stick is held by hands for a long time, so that the discomfort of the hands is increased. Harmful substances contained in the smoke can cause certain harm to smokers.
In the prior art, a filter stick of a cigarette is improved by arranging adsorbing materials such as active carbon and the like, or a bead blasting method is used, and substances released by the bead blasting method are adsorbed after the bead blasting method is pinched and broken. But the adsorption effect is limited, a certain amount of large-particle agglomerated smoke enters the mouth of a smoker through the filter stick, the filtering effect is not ideal, and the temperature of the filter stick is also high.
Disclosure of Invention
In view of the problems in the prior art, the present invention aims to provide a porous frame solid bead, a preparation method and applications thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a porous frame solid bead comprises carboxymethyl cellulose, an adsorption material and a cooling material, wherein the carboxymethyl cellulose is used as a base material and a binder, the solid bead is of a porous net structure, porous channels are formed in the solid bead, and the carboxymethyl cellulose, the adsorption material and the cooling material are composed of, by weight, 30-50 parts of carboxymethyl cellulose, 10-30 parts of the adsorption material and 20-40 parts of the cooling material.
The porous net structure of the solid bead penetrates through the whole solid bead, and the smoke passes through the solid bead.
Compared with the existing adsorbing material, the solid beads obtained by the invention have the advantages of stable structure, good adsorption effect and cooling effect. Compared with the existing adsorption material, the solid beads provided by the invention are different in that the adsorption is carried out through the porous structure, so that the agglomerated smoke in the smoke is dispersed and flows in the beads after passing through the solid beads, the smoke flowing time is prolonged, the smoke temperature is reduced, the functions of filtration, adsorption, cooling and the like are realized while the aroma is increased, and the comfort of cigarette smoking is improved.
In a second aspect, the preparation method of the porous frame solid bead is as follows: and (3) adding the adsorbing material and the cooling material into a wet mixing granulator simultaneously, granulating firstly, and then drying to obtain porous granules.
And putting the powder for granulation or the granule (powder) material for coating into a wet mixing granulator, completing the formation of encapsulated powder granules by adjusting the technological parameters such as aperture, rotating speed, temperature and the like, and finally drying to obtain the dry beads.
In a third aspect, the porous frame solid beads are used in the field of cigarettes.
In a fourth aspect, a filter rod comprises the porous frame solid bead.
In a fifth aspect, a cigarette comprises the porous frame solid beads described above.
The invention has the beneficial effects that:
the porous frame solid beads have a porous net structure, smoke contains a large amount of large particles, the smoke is in an agglomerated state, the large particles become small particles after the solid beads are filtered and adsorbed, the smoke is in a dispersed state, the smoke is more cotton and fine, and the smoking comfort of cigarettes is improved.
The porous frame solid beads can be added with various fragrance slow-release materials, the fragrance slow-release materials are soaked on the surfaces of or in the porous particles, fragrance is taken away along with the flowing of smoke, the fragrance release speed in the porous frame solid beads is low, and the porous frame solid beads have a slow-release effect.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is an SEM image of porous framed solid beads prepared in example 1;
FIG. 2 is a schematic view of smoke passing through a filter rod;
FIG. 3 is a schematic structural view of a wet mixing granulator;
the device comprises a machine body, a staircase, a stirring transmission device, a discharging device, a sandwich pot, a cover plate part, a slurry adding part, a powder scraping mechanism, a detection hole, a granulating cutter transmission device, a machine body and a powder scraping mechanism, wherein the staircase is 2, the stirring transmission device is 3, the discharging device is 4, the sandwich pot is 5, the cover plate part is 6, the slurry adding part is 7, the powder scraping mechanism is 8, the detection hole.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
A porous frame solid bead comprises carboxymethyl cellulose, an adsorption material and a cooling material, wherein the carboxymethyl cellulose is used as a base material and a binder, the solid bead is of a porous net structure, porous channels are formed in the solid bead, and the carboxymethyl cellulose, the adsorption material and the cooling material are composed of, by weight, 30-50 parts of carboxymethyl cellulose, 10-30 parts of the adsorption material and 20-40 parts of the cooling material.
According to the solid bead, the carboxymethyl cellulose is used as the base material and the binder, the carboxymethyl cellulose forms a structure with a mesh-shaped porous channel after a granulation process, the adsorption material and the cooling material are uniformly distributed in the solid bead, and when smoke passes through the solid bead, the smoke can be fully contacted with the adsorption material and the cooling material, so that the adsorption and cooling performances are improved.
The existing filter stick is added with the bead blasting, and substances released after the bead blasting is pinched off play a certain adsorption role, but the adsorption effect is limited, and the flowing state of large-particle agglomerated smoke cannot be changed.
After the tobacco is burnt, substances such as tar and the like are generated and exist in the smoke in the form of larger particles. Tar can be a cause of lung cancer and laryngeal cancer, and also can cause yellow finger and tooth of smokers. The flue gas passes through the pore channels of the solid beads after passing through the solid beads, the flowing time of the flue gas is prolonged due to the complex pore channels, large particles such as tar are gradually partially adsorbed to become small particles, and the flue gas needs to pass through a plurality of pore channels, so that the flue gas is dispersed.
In some embodiments of the invention, an aroma slow release material is also included.
Further, the aroma slow-release material is oil-soluble or water-soluble essence and natural spice substances; furthermore, the natural perfume material is perfume with tranquilizing effect such as lavender, herba Menthae, herba Salvia officinalis, fructus Anisi Stellati, etc., perfume with diuretic effect such as juniper, lavender, Bulbus Allii Cepae, herba Thymi vulgaris, etc., perfume with stomach invigorating effect such as rhizoma Zingiberis recens, flos Caryophylli, herba Menthae, Bulbus Allii Cepae, herba Rosmarini officinalis, etc., and perfume with pathogenic wind expelling effect such as flos Caryophylli, Achyranthis radix, fructus Citri Limoniae, etc.
The porous particle structure of the invention is also beneficial to releasing aroma in smoke, and when the smoke flows in the porous structure of the porous particle, the smoke is more fully contacted with the aroma, and the aroma is more fully released.
In some embodiments of the invention, the weight ratio of the carboxymethyl cellulose to the adsorbing material to the cooling material to the fragrance slow-release material is 5-7:1-3:1: 1; preferably, the weight ratio is 6:2:1: 1.
In some embodiments of the invention, the adsorbent material is graphene, diatomaceous earth or MOFs material. Graphite has a special surface structure and a high specific surface area. Diatomaceous earth has a high specific surface area. The MOFs material is a Metal Organic Framework (MOFs) material with central metal ions combined with organic ligands, and has the characteristic of capturing various heavy metal substances.
In some embodiments of the invention, the cooling material is a clay or a silica gel.
The two substances are selected as the adsorbent, so that the adsorbent has the advantages of good adsorption effect and large adsorption capacity, and has the property of forming a stable porous particle structure with a cooling material, if other substances are selected for combination, the obtained porous structure is unstable or has poor effect, and the argil can be used as a filter aid and an adsorbent for removing a heat source. The silica gel is hard gel with a net structure, has rich pore passages, large specific surface area, stable chemical property, no toxicity, no odor and high temperature resistance, and simultaneously has the functions of moisture retention and adsorption. The pottery clay and the silica gel can meet the requirement of solid bead particles for cigarettes on mechanical strength, and can reduce the temperature and increase the moisture of smoke to a certain extent and adsorb the smoke.
In a second aspect, the preparation method of the porous frame solid bead is as follows: and (3) simultaneously adding the adsorbing material and the cooling material into a wet mixing granulator, simultaneously adding carboxymethyl cellulose, granulating and drying to obtain the porous frame solid beads.
In some embodiments of the invention, the feed rate in the fluid bed granulation stage is 0.5-1.0 kg/batch and the feed rate in the drying stage is 0.3-0.7 kg/batch; preferably, the amount fed in the fluid bed granulation stage is 0.6-0.8 kg/batch and the amount fed in the drying stage is 0.5-0.6 kg/batch.
In some embodiments of the invention, the fan power during the drying stage is between 0.7 and 0.8 kw.
In some embodiments of the invention, the speed of the granulating blade is 30-150r/min, and the size of the resulting porous granules can be controlled by adjusting the speed of the granulating blade.
In some embodiments of the invention, the temperature of the hot air in the drying stage is 80-200 ℃; preferably 100-.
In some embodiments of the present invention, after the raw material is prepared by a wet mixing granulator to obtain the composite material, the porous framework solid beads with a circular structure are obtained by rounding treatment.
In some embodiments of the present invention, the prepared porous framework solid beads are mixed with a fragrance slow-release material, and a swelling agent is added during the mixing process, and after the mixing, microwave expansion treatment is performed to obtain fragrance-loaded porous particles. Further, the leavening agent is sodium bicarbonate, disodium dihydrogen pyrophosphate, calcium hydrogen phosphate or calcium carbonate. The volume of the pore channel can be increased by the microwave expansion treatment.
In a third aspect, the porous frame solid beads are used in the field of cigarettes.
In a fourth aspect, a filter rod comprises the porous frame solid bead.
In a fifth aspect, a cigarette comprises the porous frame solid beads described above.
The invention will be further illustrated by the following examples
Example 1
Feeding carboxymethyl cellulose, an adsorption material and a cooling material serving as raw materials into a feeding port of a wet mixing granulator, granulating in the wet mixing granulator, and then performing rounding and drying treatment to obtain porous particles, wherein the adsorption material is graphene and the cooling material is argil;
the specific treatment steps are as follows: adding an adsorbing material and a cooling material into a jacketed kettle of the mixing granulator, and then closing the cover plate part to seal the jacketed kettle; and opening the transmission system to enable the stirring knife and the plasmid knife to start rotating, and simultaneously injecting the carboxymethyl cellulose solution into the jacketed kettle by the slurry adding mechanism to start the granulation process. The plasmid process of each batch of products is about 20-30 minutes, the plasmid condition is checked through the inspection hole, after the plasmid is finished, the transmission system is closed, and the prepared porous frame solid beads are taken out through the discharging device. Then putting the solid beads into a spheronization drying pan for about 30-40 minutes to obtain finished product porous frame solid beads. The carboxymethyl cellulose solution is a mixture of carboxymethyl cellulose and water, and is dried after granulation.
As shown in FIG. 3, the model of the wet mixing granulator is GHL-50 type high-efficiency wet mixing granulator, and the manufacturer is constant mechanical manufacturing company Limited in Jiangyin. The external dimension L multiplied by W multiplied by H of the main machine of the wet mixing granulator is about 650 multiplied by 1000 multiplied by 1300 mm; the machine body 10 is provided with the escalator 1, the stirring transmission 2 is used for transmission of the stirring mechanism, and the granulating cutter transmission 9 controls the stirring cutter and the plasmid cutter to rotate. The inspection hole 8 is used for checking plasmid conditions, the powder scraping mechanism 7 is used for discharging, the slurry adding part 6 is used for adding carboxymethyl cellulose, the cover plate part 5 covers the top of the granulator, the jacketed pan 4 is the main granulating position, and the discharging device 3 is used for outputting materials.
Controlling the feeding amount to be 0.6 kg/batch in the fluidized bed granulation process, and controlling the feeding amount to be 0.5 kg/batch in the drying stage; the fan power of the hot air is 0.75kw (variable frequency speed regulation); the electric heating power of the hot air is 1.5 KW; electrically controlling the PLC and the touch screen; the weight of the apparatus was about 350 (Kg).
The rounding equipment was a JW extrusion spheronizer-extrusion shot-blasting machine, the manufacturer was Tokyo Torpedo drying equipment, Inc., and the overall dimensions (length. times. width. times. height) were about 1100X 550. times.1300 mm.
The SEM image of the solid beads with porous frame obtained in example 1 is shown in fig. 1, and it can be seen that the surface of the solid beads with porous frame has a porous structure.
The wet mixing granulator can be equipment of other types or models, and realizes the mixing granulation and drying processes of the carboxymethyl cellulose, the adsorption material and the cooling material.
Example 2
Feeding carboxymethyl cellulose, an adsorption material and a cooling material serving as raw materials into a feeding port of a multifunctional boiling granulation dryer, and sequentially performing granulation and drying treatment steps in the multifunctional boiling granulation dryer to obtain porous particles, wherein the adsorption material is diatomite and the cooling material is silica gel;
the wet mixing granulator was the same as in example 1; the difference is that: the amount of feed in the fluid bed granulation process was controlled to 0.8 kg/batch and the amount of feed in the drying stage was controlled to 0.7 kg/batch.
Comparative example
Unlike example 1, no kaolin was added.
Test examples
The porous frame solid beads obtained in examples 1 and 2 were placed in a filter rod during the production of the filter rod, and a smoke filtration experiment was performed. The process of smoke passing through the filter stick is shown in figure 2, and large-particle agglomerated smoke is filtered and adsorbed to form small-particle filtered smoke.
40 cigarettes without any particulate matter added were divided into 2 batches of 4 groups of 5 cigarettes each, and equilibrated for 48h at a temperature (22 + -1 deg.C) and a relative humidity (60 + -3)%.
Putting the 1 st batch of 20 cigarettes into a 20-channel turntable type smoking machine to perform a smoke total particulate matter test, wherein the result is the content of the smoke total particulate matter before adsorption;
replacing the 2 nd batch of 20 filter tips of cigarettes with the filter tips prepared by the comparative example 1, the example 2 and the activated carbon respectively, and then putting the filter tips into a 20-channel turntable type smoking machine for testing the total particulate matters in the smoke, wherein the result is the content of the total particulate matters in the smoke after adsorption;
the smoke before and after filtration was measured to obtain the results shown in table 1, wherein the activated carbon means that the same mass of activated carbon as that of the solid beads of example 1 was added to the filter rod.
TABLE 1 filtration Effect of different solid beads
Figure BDA0002525862500000081
By comparing comparative example 1 with examples 1 and 2, it is shown that if kaolin is added, the adsorption performance of the solid beads is improved, and in the comparative example, no kaolin is added, the obtained solid beads are easy to be broken by kneading, and the porous channel structure is damaged.
The comparison between the activated carbon and the examples 1 and 2 shows that the solid beads of the invention have better adsorption and temperature reduction effects.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A porous frame solid bead characterized by: the solid bead is in a porous net structure, porous channels are formed in the solid bead, and the carboxymethyl cellulose, the adsorbing material and the cooling material are composed of, by weight, 30-50 parts of carboxymethyl cellulose, 10-30 parts of the adsorbing material and 20-40 parts of the cooling material.
2. The porous frame solid bead of claim 1, wherein: also comprises a fragrance slow-release material;
preferably, the aroma slow-release material is oil-soluble or water-soluble essence and natural spice substances;
further preferably, the natural spice is lavender, peppermint, sage, anise, juniper, lavender, onion, thyme, ginger, clove, peppermint, onion, rosemary, clove, hyssop, lemon.
3. The porous frame solid bead of claim 2, wherein: the weight ratio of the carboxymethyl cellulose to the adsorbing material to the cooling material to the fragrance slow-release material is 5-7:1-3:1: 1; preferably, the weight ratio is 6:2:1: 1.
4. The porous frame solid bead of claim 1, wherein: the adsorbing material is graphene or diatomite.
5. The porous frame solid bead of claim 1, wherein: the cooling material is pottery clay or silica gel.
6. A method of preparing porous framed solid beads according to any of claims 1 to 5, characterized in that: the method comprises the following steps: and (3) simultaneously adding the adsorbing material and the cooling material into a wet mixing granulator, simultaneously adding carboxymethyl cellulose, granulating and drying to obtain the porous frame solid beads.
7. The method of preparing porous frame solid beads of claim 6, wherein: the feeding amount in the fluidized bed granulation stage is 0.5-1.0 kg/batch, and the feeding amount in the drying stage is 0.3-0.7 kg/batch; preferably, the amount of feed in the fluid bed granulation stage is 0.6-0.8 kg/batch, and the amount of feed in the drying stage is 0.5-0.6 kg/batch;
or the fan power in the drying stage is 0.7-0.8 kw;
or the rotating speed of the granulating cutter is 30-150 r/min;
or the temperature of hot air in the drying stage is 80-200 ℃; preferably 100-150 ℃;
or, after the raw materials are prepared into the composite material by a wet mixing granulator, rounding to obtain porous frame solid beads with a circular structure;
or mixing the prepared porous frame solid beads with the fragrance slow-release material, adding a swelling agent in the mixing process, and performing microwave expansion treatment after mixing to obtain fragrance-loaded porous particles; preferably, the leavening agent is sodium bicarbonate, disodium dihydrogen pyrophosphate, calcium hydrogen phosphate or calcium carbonate.
8. Use of porous frame solid beads according to any one of claims 1 to 5 in the field of cigarettes.
9. A filter stick is characterized in that: comprising solid beads of a porous framework as claimed in any one of claims 1 to 5.
10. A cigarette, characterized by: comprising solid beads of a porous framework as claimed in any one of claims 1 to 5.
CN202010503989.3A 2020-06-05 2020-06-05 Porous frame solid bead and preparation method and application thereof Pending CN111789286A (en)

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Publication number Priority date Publication date Assignee Title
CN112754069A (en) * 2020-12-11 2021-05-07 贵州中烟工业有限责任公司 Cigarette bead with rotary flavoring function and filter

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CN110013806A (en) * 2019-04-17 2019-07-16 云南中烟工业有限责任公司 A kind of porous complex microsphere of graphene-plant and the preparation method and application thereof
CN110754688A (en) * 2019-11-11 2020-02-07 云南恩典科技产业发展有限公司 Fragrant bead capable of pinching and breaking hollow large-particle filter stick and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112754069A (en) * 2020-12-11 2021-05-07 贵州中烟工业有限责任公司 Cigarette bead with rotary flavoring function and filter

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Application publication date: 20201020