CN105688830B - Residue porous material and application thereof after a kind of fragrant plant extraction - Google Patents

Residue porous material and application thereof after a kind of fragrant plant extraction Download PDF

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Publication number
CN105688830B
CN105688830B CN201610104980.9A CN201610104980A CN105688830B CN 105688830 B CN105688830 B CN 105688830B CN 201610104980 A CN201610104980 A CN 201610104980A CN 105688830 B CN105688830 B CN 105688830B
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residue
fragrant plant
porous material
cigarette
extraction
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CN105688830A (en
Inventor
张玲
曾晓鹰
张天栋
胡魏耀
高锐
汤丹瑜
雷声
杨建云
赵蔚
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China Tobacco Yunnan Industrial Co Ltd
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China Tobacco Yunnan Industrial Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • A24D3/14Use of materials for tobacco smoke filters of organic materials as additive
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

The preparation method of residue porous material after being extracted the invention discloses a kind of fragrant plant;Residue porous material is used to mix in cigarette filter with the purposes to cigarette smoke reducing tar and reducing harm and/or increase flue gas moist feeling after being extracted simultaneously the invention also discloses fragrant plant.

Description

Residue porous material and application thereof after a kind of fragrant plant extraction
Technical field
Residue porous material and application thereof, belongs to cigarette mouth stick added material after being extracted the present invention relates to a kind of fragrant plant Technical field.
Background technology
The operation that solvent extraction is carried out to fragrant plant, such as water extraction or alcohol are frequently involved in essence and flavoring agent processing industry Extraction, these extraction operations generate the residue after the extraction of substantial amounts of fragrant plant, it is necessary to which effective method handles these waste materials.
Also it is look for effectively adsorbing the harmful substances such as the tar in cigarette smoke in tobacco business to realize that tar reduction subtracts The material of evil effect.Filter-tip material conventional in tobacco business is acetate silk at present, though it can effective tar adsorption Substances are waited, but also have shortcoming, the cigarette smoke after being filtered shows slightly " drying ", influences mouthfeel.
It is of the invention then residual after Particular craft prepares fragrant plant extraction as raw material by residue after being extracted using fragrant plant Slag porous material, and apply it in cigarette filter, solve the problems, such as flue gas drying.
The content of the invention
The first aspect of the present invention is to provide residue porous material after a kind of fragrant plant is extracted, following by including It is prepared by the method for step:
(1) residue carries out microwave treatment after fragrant plant is extracted, the condition of the microwave treatment for microwave power 350~ 750W, microwave treatment time are 5~20min, then rear residue are taken to be dried at 70~110 DEG C the fragrant plant after microwave treatment It does to constant weight;
(2) by step (1) obtained material using mass ratio as 1:2~1:6 ratio is mixed with KOH solid powders, With the heating rate of 5~20 DEG C/min to 500~700 DEG C in argon atmosphere, 10~30min is kept at this temperature;
(3) material that step (2) obtains with the HCl that concentration is 5%~15% is cleaned and removes KOH, then use distilled water After cleaning is neutral to pH value, the porous material of residue after being extracted to the fragrant plant is dried to constant weight at 100~150 DEG C Material.
Residue is residue of the fragrant plant after water extraction or alcohol extracting after wherein described fragrant plant extraction.For example, It may particularly include following several:The water extract residue of single variety, the alcohol extract residue of single variety, two kinds and more than it is compound Be formulated water extract residue, two kinds and more than compound prescription alcohol extract residue.
Wherein described fragrant plant is selected from rose, peppermint, rosemary, tribute chrysanthemum, the lily of the valley, cloud safflower, tree orchid, violet, smokes One or more of clothing grass, Tibet inula root.
Preferably, after step (1), also raw material is crushed and screened to obtain 20~80 mesh powders.
Second aspect of the present invention be related to after aforementioned fragrance plant extract residue porous material for mix in cigarette filter with To the purposes of cigarette smoke reducing tar and reducing harm and/or increase flue gas moist feeling.
Preferably, after the fragrant plant extraction incorporation of the residue porous material in cigarette filter for 15mg~ 30mg/ branch.
Beneficial effects of the present invention:
(1) residue porous material has porous performance after fragrant plant of the invention extraction, has larger specific surface area, Average pore size is moderate, meets the feature requirement of filter stick sorbing material, and therefore, which there is retention well to be adsorbed with The effect of evil object, can keep having different degrees of reducing tar and reducing harm effect while original style is constant to kinds of cigarettes in cigarette.
(2) residue porous material is nontoxic after fragrant plant extraction, and source is sufficient, and technological process is simple, making side Just, of low cost, addition is simple, does not change existing cigarette producing process;
(3) residue porous material realizes fragrant plant extract residue and effectively makes full use of after fragrant plant is extracted;
(4) have been surprisingly found that, residue porous material can improve cigarette smoke after filter tip is mixed after fragrant plant extraction Moist feeling, be effectively improved cigarette comfort.
Specific embodiment
With reference to the present invention is described in further detail with embodiment, but protection scope of the present invention is not limited to The content.
Embodiment 1
Residue after fragrant plant extraction described in the present embodiment, using rosemary as raw material it is extracted after residual residue filtered, Then material after microwave treatment at 50 DEG C is dried, sieved after crushed by the microwave treatment 15min under the microwave power of 350W Obtain 20 mesh powders.
The preparation method of residue porous material, specifically includes following steps after fragrant plant extraction of the present invention:By 20 Purpose Rosmarinus officinalis extract residue powder, by it using mass ratio as 1:3 ratio is put into tube furnace jointly with KOH solid powders In, with the heating rate of 10 DEG C/min to 500 DEG C under argon atmosphere, 15min is kept the temperature, is then cleaned with the HCl that concentration is 5% KOH is removed, it is neutral to be cleaned with distilled water to pH value, and finally material dries to constant weight at 110 DEG C.
Specific standard tow is selected, porous material is subjected to charge bar on KDF-2E forming machines and is rolled, selects specification tow White stick is rolled on KDF-2E forming machines, charge bar carries out composite molding with white stick on composite molding machine, it is compound to roll into binary Filter stick, recombination length 1:1;Additive amount of the porous material in mouth stick is 15mg/ branch.
Then by smoke panel test panel of expert by《The requirement of GB5606.4-1996 cigarette sense organs technology》Regulation carry out cigarette sense organ It smokes panel test.Control sample is not add in the normal cigarette of porous material, and smoking result is shown in Table 1.Smoking result in table 1 shows the virtue Residue porous material can reduce irritation after fragrant plant extract, moist feeling be improved, to cigarette sensory quality without negative effect.
1 cigarette sensory evaluating smoking's result of table
Further to analyze porous material absorption effect, according to the relevant criterion of GB 5606.5-2005 to the master of cigarette Stream flue gas is routinely analyzed, and the results are shown in Table 2, result is the average value after survey three times.Table 2 the result shows that, the porous material pair Cigarette smoke index is without negative effect, and wherein tar content and CO contents decreases, and moisture has unexpected raising.
2 composite filter tip cigarette conventional index of table detects
Embodiment 2
Residue after fragrant plant extraction described in the present embodiment, using lavender as raw material it is extracted after residual residue filtered, The microwave treatment 10min under the microwave power of 500W, then in 50 DEG C of drying, screening after crushed obtains 40 mesh powders.
The preparation method of residue porous material, specifically includes following steps after fragrant plant extraction of the present invention:By 40 Residue powder is using mass ratio as 1 after the extraction of purpose lavender:2 ratio is put into tube furnace jointly with KOH solid powders, in argon Atmosphere enclose under with the heating rate of 20 DEG C/min to 700 DEG C, keep the temperature 10min, then clean removal with concentration for 10% HCl KOH, it is neutral to be cleaned with distilled water to pH value, and finally material dries to constant weight at 150 DEG C.
Specific standard tow is selected, porous material is subjected to charge bar on KDF-2E forming machines and is rolled, selects specification tow White stick is rolled on KDF-2E forming machines, charge bar carries out composite molding with white stick on composite molding machine, it is compound to roll into binary Filter stick, recombination length 1:1;Additive amount of the porous material in mouth stick is 20mg/ branch.
Then by smoke panel test panel of expert by《The requirement of GB5606.4-1996 cigarette sense organs technology》Regulation carry out cigarette sense organ It smokes panel test.Control sample is not add in the normal cigarette of porous material, and smoking result is shown in Table 3.Smoking result in table 3 shows that this is more Porous materials can make cigarette perfume finer and smoother, and reducing stimulates, and not change original style and features of cigarette.
3 cigarette sensory evaluating smoking's result of table
Further to analyze porous material absorption effect, according to the relevant criterion of GB 5606.5-2005 to the master of cigarette Stream flue gas is routinely analyzed, and the results are shown in Table 4, result is the average value after survey three times.Table 4 the result shows that, the porous material pair Cigarette smoke index is without negative effect, and wherein tar content and CO contents decreases, and moisture has unexpected raising.
4 composite filter tip cigarette conventional index of table detects
Embodiment 3
Residue after fragrant plant extraction described in the present embodiment, by raw material violet, lavender it is extracted after by residual residue Then filtering, the microwave treatment 5min under the microwave power of 700W dry the material after microwave treatment at 70 DEG C, after crushed Screening obtains 60 mesh powders.
The preparation method of residue porous material, specifically includes following steps after fragrant plant extraction of the present invention:By 60 Purpose violet, Herba Lysimachiae foenumgraeci extract residue powder are using mass ratio as 1:6 ratio is put into tube furnace jointly with KOH solid powders In, with the heating rate of 15 DEG C/min to 600 DEG C under argon atmosphere, 20min is kept the temperature, it is then clear with the HCl that concentration is 15% It washes away except KOH, it is neutral to be cleaned with distilled water to pH value, and finally material dries to constant weight at 120 DEG C.
Specific standard tow is selected, porous material is subjected to charge bar on KDF-2E forming machines and is rolled, selects specification tow White stick is rolled on KDF-2E forming machines, charge bar carries out composite molding with white stick on composite molding machine, it is compound to roll into binary Filter stick, recombination length 1:1;Additive amount of the porous material in mouth stick is 25mg/ branch.
Then by smoke panel test panel of expert by《The requirement of GB5606.4-1996 cigarette sense organs technology》Regulation carry out cigarette sense organ It smokes panel test.Control sample is not add in the normal cigarette of porous material, and smoking result is shown in Table 3.Smoking result in table 3 shows that this is more Porous materials can make cigarette perfume finer and smoother, and reducing stimulates, and not change original style and features of cigarette.
3 cigarette sensory evaluating smoking's result of table
Further to analyze porous material absorption effect, according to the relevant criterion of GB 5606.5-2005 to the master of cigarette Stream flue gas is routinely analyzed, and the results are shown in Table 4, result is the average value after survey three times.Table 4 the result shows that, the porous material pair Cigarette smoke index is without negative effect, and wherein tar content and CO contents decreases, and moisture has unexpected raising.
4 composite filter tip cigarette conventional index of table detects
Embodiment 4
Described in the present embodiment fragrant plant extraction after residue porous material, by raw material tribute chrysanthemum, the lily of the valley, cloud safflower it is extracted after Residual residue is filtered, the microwave treatment 15min under the microwave power of 400W, then by the material after microwave treatment in 80 DEG C of bakings Dry, screening after crushed obtains 40 mesh powders.
The preparation method of residue porous material, specifically includes following steps after fragrant plant extraction of the present invention:By 40 Purpose tribute chrysanthemum, the lily of the valley, cloud safflower extract residue powder are using mass ratio as 1:5 ratio is put into pipe jointly with KOH solid powders In formula stove, with the heating rate of 10 DEG C/min to 650 DEG C under argon atmosphere, 30min is kept the temperature, is then 12% with concentration HCl cleaning removal KOH, it is neutral to be cleaned with distilled water to pH value, and finally material dries to constant weight at 130 DEG C.
Specific standard tow is selected, porous material is subjected to charge bar on KDF-2E forming machines and is rolled, selects specification tow White stick is rolled on KDF-2E forming machines, charge bar carries out composite molding with white stick on composite molding machine, it is compound to roll into binary Filter stick, recombination length 1:1;Additive amount of the porous material in mouth stick is 30mg/ branch.
Then by smoke panel test panel of expert by《The requirement of GB5606.4-1996 cigarette sense organs technology》Regulation carry out cigarette sense organ It smokes panel test.Control sample is not add in the normal cigarette of porous material, and smoking result is shown in Table 3.Smoking result in table 3 shows that this is more Porous materials can make cigarette perfume finer and smoother, and reducing stimulates, and not change original style and features of cigarette.
3 cigarette sensory evaluating smoking's result of table
Further to analyze porous material absorption effect, according to the relevant criterion of GB 5606.5-2005 to the master of cigarette Stream flue gas is routinely analyzed, and the results are shown in Table 4, result is the average value after survey three times.Table 4 the result shows that, the porous material pair Cigarette smoke index is without negative effect, and wherein tar content and CO contents decreases, and moisture has unexpected raising.
4 composite filter tip cigarette conventional index of table detects
Embodiment 5
Residue porous material after fragrant plant extraction described in the present embodiment, with Tibet inula root, tribute chrysanthemum, the lily of the valley, cloud safflower, rose Residual residue is filtered after extracted, the microwave treatment 9min under the microwave power of 660W, then by the material after microwave treatment In 90 DEG C of drying, screening after crushed obtains 80 mesh powders.
The preparation method of residue porous material, specifically includes following steps after fragrant plant extraction of the present invention:By 80 Purpose Tibet inula root, tribute chrysanthemum, the lily of the valley, cloud safflower, rose extract residue powder are using mass ratio as 1:4 ratio and KOH solid powder End is put into tube furnace jointly, with the heating rate of 10 DEG C/min to 600 DEG C under argon atmosphere, 20min is kept the temperature, then with dense The HCl cleaning removal KOH for 15% are spent, it is neutral to be cleaned with distilled water to pH value, and material finally is dried to perseverance at 150 DEG C Weight.
Specific standard tow is selected, porous material is subjected to charge bar on KDF-2E forming machines and is rolled, selects specification tow White stick is rolled on KDF-2E forming machines, charge bar carries out composite molding with white stick on composite molding machine, it is compound to roll into binary Filter stick, recombination length 1:1;Additive amount of the porous material in mouth stick is 20mg/ branch.
Then by smoke panel test panel of expert by《The requirement of GB5606.4-1996 cigarette sense organs technology》Regulation carry out cigarette sense organ It smokes panel test.Control sample is not add in the normal cigarette of porous material, and smoking result is shown in Table 3.Smoking result in table 3 shows that this is more Porous materials can make cigarette perfume finer and smoother, and reducing stimulates, and not change original style and features of cigarette.
3 cigarette sensory evaluating smoking's result of table
Further to analyze porous material absorption effect, according to the relevant criterion of GB 5606.5-2005 to the master of cigarette Stream flue gas is routinely analyzed, and the results are shown in Table 4, result is the average value after survey three times.Table 4 the result shows that, the porous material pair Cigarette smoke index is without negative effect, and wherein tar content and CO contents decreases, and moisture has unexpected raising.
4 composite filter tip cigarette conventional index of table detects

Claims (4)

1. after a kind of extraction of fragrant plant residue porous material for mix in cigarette filter with to cigarette smoke reducing tar and reducing harm and/ Or increase the purposes of flue gas moist feeling, which is characterized in that residue porous material is following by including after the fragrant plant extraction It is prepared by the method for step:
(1) residue carries out microwave treatment after fragrant plant is extracted, the condition of the microwave treatment for microwave power 350~ 750W, microwave treatment time are 5~20min, then by residue after the fragrant plant extraction after microwave treatment at 70~110 DEG C It is lower that drying to constant weight;
(2) by step (1) obtained material using mass ratio as 1:2~1:6 ratio is mixed with KOH solid powders, in argon gas With the heating rate of 5~20 DEG C/min to 500~700 DEG C in atmosphere, 10~30min is kept at this temperature;
(3) material that step (2) obtains with the HCl that concentration is 5%~15% is cleaned and removes KOH, then cleaned with distilled water After being neutral to pH value, residue porous material after being extracted to the fragrant plant is dried to constant weight at 100~150 DEG C.
2. purposes according to claim 1, which is characterized in that residue is fragrant plant after wherein described fragrant plant extraction Residue after water extraction or alcohol extracting.
3. purposes according to claim 2, which is characterized in that wherein described fragrant plant changes selected from rose, peppermint, fan One or more of perfume, tribute chrysanthemum, the lily of the valley, cloud safflower, tree orchid, violet, lavender, Tibet inula root.
4. purposes according to claim 1, which is characterized in that residue porous material is in cigarette after the fragrant plant extraction Incorporation in filter tip is 15mg~30mg/ branch.
CN201610104980.9A 2016-02-25 2016-02-25 Residue porous material and application thereof after a kind of fragrant plant extraction Active CN105688830B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837975A (en) * 2010-05-20 2010-09-22 湖南太和科技有限公司 Microwave complex activation method for preparing super porous carbon
CN103803548A (en) * 2014-02-20 2014-05-21 江西师范大学 Biomass powder activated carbon prepared from lychee seeds and preparation method thereof
CN104140101A (en) * 2014-08-18 2014-11-12 福建师范大学 Method for preparing activated carbon with ultrahigh specific surface area from soapberry residue as raw material
CN104386691A (en) * 2014-10-21 2015-03-04 北京科技大学 Method for preparing hollow tubular activated carbon electrode material for supercapacitor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837975A (en) * 2010-05-20 2010-09-22 湖南太和科技有限公司 Microwave complex activation method for preparing super porous carbon
CN103803548A (en) * 2014-02-20 2014-05-21 江西师范大学 Biomass powder activated carbon prepared from lychee seeds and preparation method thereof
CN104140101A (en) * 2014-08-18 2014-11-12 福建师范大学 Method for preparing activated carbon with ultrahigh specific surface area from soapberry residue as raw material
CN104386691A (en) * 2014-10-21 2015-03-04 北京科技大学 Method for preparing hollow tubular activated carbon electrode material for supercapacitor

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