CN105688830A - Porous material made of residues obtained after extraction of aromatic plants and application of porous material - Google Patents

Porous material made of residues obtained after extraction of aromatic plants and application of porous material Download PDF

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Publication number
CN105688830A
CN105688830A CN201610104980.9A CN201610104980A CN105688830A CN 105688830 A CN105688830 A CN 105688830A CN 201610104980 A CN201610104980 A CN 201610104980A CN 105688830 A CN105688830 A CN 105688830A
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China
Prior art keywords
porous material
residue
fragrant plant
extraction
extracted
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CN201610104980.9A
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CN105688830B (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 invention discloses a preparation method of a porous material made of residues obtained after extraction of aromatic plants and meanwhile further discloses application of the porous material made of the residues obtained after extraction of the aromatic plants that the material is mixed into cigarette filter tips so that tar and other harmful components in cigarettes can be reduced and/or moistening feeling of smoke can be enhanced.

Description

Residue porous material and application thereof after a kind of fragrant plant extraction
Technical field
The present invention relates to residue porous material and application thereof after a kind of fragrant plant is extracted, belong to cigarette mouth rod adding material technical field。
Background technology
Frequently involving the operation that fragrant plant carries out solvent extraction in essence and flavoring agent processing industry, for instance water extraction or alcohol extraction, these extract operation and produce the residue after substantial amounts of fragrant plant is extracted, it is necessary to effective method processes these waste materials。
Tobacco business is also look for can the harmful substance such as tar in active adsorption cigarette smoke to realize the material of reducing tar and reducing harm effect。Filter-tip material conventional in current tobacco business is acetate silk, though the materials such as its energy active adsorption tar, but also have weak point, the cigarette smoke after being filtered shows slightly " drying ", affects mouthfeel。
The present invention then prepares fragrant plant extract after residue porous material for raw material through Particular craft by residue after extracting with fragrant plant, and applies it in cigarette filter, solves flue gas drying problem。
Summary of the invention
A first aspect of the present invention be in that to provide a kind of fragrant plant to extract after residue porous material, it is prepared by the method comprised the following steps:
(1) after being extracted by fragrant plant, residue carries out microwave treatment, the condition of described microwave treatment is microwave power 350~750W, microwave treatment time is 5~20min, then the fragrant plant after microwave treatment is taken rear residue and dries to constant weight at 70~110 DEG C;
(2) material obtained for step (1) is mixed with KOH pressed powder with the ratio that mass ratio is 1:2~1:6, with the programming rate of 5~20 DEG C/min to 500~700 DEG C in argon atmosphere, keep 10~30min at this temperature;
(3) HCl that material concentration is 5%~15% step (2) obtained cleans and removes KOH, then clean after being neutrality to pH value with distilled water, dry to constant weight at 100~150 DEG C, namely obtain residue porous material after described fragrant plant is extracted。
After wherein said fragrant plant is extracted, residue is fragrant plant residue after water extraction or alcohol extraction。Such as, may particularly include following several: the water extract residue of single variety, the ethanol extract residue of single variety, two kinds and above compound prescription water extract residue, two kinds and above compound prescription ethanol extract residue。
Wherein said fragrant plant selected from Flos Rosae Rugosae, Herba Menthae, Herba Rosmarini Officinalis, Flos Chrysanthemi, Herba Convallariae, cloud Flos Carthami, tree orchid, violet, lavandula angustifolia, one or more in Radix Inulae。
Preferably, after step (1), also raw material pulverizing screening is obtained the powder of 20~80 orders。
Second aspect present invention relate to aforementioned fragrance plant extract after residue porous material for mix in cigarette filter with to cigarette smoke reducing tar and reducing harm and/or increase flue gas moist feeling purposes。
Preferably, after described fragrant plant is extracted, residue porous material incorporation in cigarette filter is that 15mg~30mg/ props up。
Beneficial effects of the present invention:
(1) after the fragrant plant of the present invention is extracted, residue porous material has porous performance, there is bigger specific surface area, average pore size is moderate, meet the feature requirement of filter stick adsorbing material, therefore, this porous material has and well retains the effect being adsorbed with pest, and kinds of cigarettes can have reducing tar and reducing harm effect in various degree while Medicated cigarette keeps original style constant。
(2) after this fragrant plant is extracted, residue porous material is nontoxic, source abundance, and technological process is simple, easy to make, with low cost, adds simple, does not change existing cigarette producing process;
(3) after fragrant plant is extracted, residue porous material achieves fragrant plant extract residue and effectively makes full use of;
(4) having been surprisingly found that, after the extraction of this fragrant plant, residue porous material can improve the moist feeling of cigarette smoke after mixing filter plug, is effectively improved Medicated cigarette comfortableness。
Detailed description of the invention
Below in conjunction with the present invention is described in further detail with embodiment, but protection scope of the present invention is not limited to described content。
Embodiment 1
Fragrant plant described in the present embodiment extract after residue, with Herba Rosmarini Officinalis for raw material extracted after residual residue is filtered, microwave treatment 15min under the microwave power of 350W, then by the material after microwave treatment 50 DEG C of drying, sieve the powder obtaining 20 orders after crushed。
The preparation method of residue porous material after fragrant plant of the present invention extraction, specifically include following steps: by the Herba Rosmarini Officinalis extract residue powder of 20 orders, it is put in tube furnace with the ratio that mass ratio is 1:3 jointly with KOH pressed powder, with the programming rate of 10 DEG C/min to 500 DEG C under argon atmosphere, insulation 15min, cleaning with the HCl that concentration is 5% subsequently and remove KOH, it is neutral for cleaning to pH value with distilled water, is finally dried to constant weight at 110 DEG C by material。
Select specific standard tow, porous material carrying out charge bar on KDF-2E forming machine roll, select specification tow to roll white rod on KDF-2E forming machine, charge bar carries out composite molding with white rod on composite molding machine, rolling into binary compound filter candle, recombination length is 1:1;This porous material addition in mouth rod is that 15mg/ props up。
Then Medicated cigarette sensory evaluating smoking is carried out by panel of expert of smokeing panel test by the regulation of " GB5606.4-1996 Medicated cigarette sense organ technology requirement "。Control sample is do not add the normal Medicated cigarette of porous material, and smoking result is in Table 1。Smoking result in table 1 shows, after this fragrant plant is extracted, residue porous material can reduce zest, improves moist feeling, to cigarette sensory quality without negative effect。
Table 1 Medicated cigarette sensory evaluating smoking's result
For analyzing this porous material absorption effect further, according to the relevant criterion of GB5606.5-2005, the main flume of Medicated cigarette being commonly performed analysis, result is in Table 2, and result is the meansigma methods after surveying three times。Table 2 it is shown that this porous material to cigarette smoke index without negative effect, wherein tar content and CO content decrease, and moisture has unexpected raising。
Table 2 composite filter tip Medicated cigarette conventional index detects
Embodiment 2
Fragrant plant described in the present embodiment extract after residue, with lavandula angustifolia for raw material extracted after residual residue is filtered, microwave treatment 10min under the microwave power of 500W, then 50 DEG C of drying, sieve after crushed and obtain the powder of 40 orders。
The preparation method of residue porous material after fragrant plant of the present invention extraction, specifically include following steps: after being extracted by the lavandula angustifolia of 40 orders, residue powder is put in tube furnace with the ratio that mass ratio is 1:2 jointly with KOH pressed powder, with the programming rate of 20 DEG C/min to 700 DEG C under argon atmosphere, insulation 10min, clean with the HCl that concentration is 10% subsequently and remove KOH, it is neutral for cleaning to pH value with distilled water, is finally dried to constant weight at 150 DEG C by material。
Select specific standard tow, porous material carrying out charge bar on KDF-2E forming machine roll, select specification tow to roll white rod on KDF-2E forming machine, charge bar carries out composite molding with white rod on composite molding machine, rolling into binary compound filter candle, recombination length is 1:1;This porous material addition in mouth rod is that 20mg/ props up。
Then Medicated cigarette sensory evaluating smoking is carried out by panel of expert of smokeing panel test by the regulation of " GB5606.4-1996 Medicated cigarette sense organ technology requirement "。Control sample is do not add the normal Medicated cigarette of porous material, and smoking result is in Table 3。Smoking result in table 3 shows, this porous material can make cigarette perfume (or spice) finer and smoother, reduces and stimulates, does not change original style and features of Medicated cigarette。
Table 3 Medicated cigarette sensory evaluating smoking's result
For analyzing this porous material absorption effect further, according to the relevant criterion of GB5606.5-2005, the main flume of Medicated cigarette being commonly performed analysis, result is in Table 4, and result is the meansigma methods after surveying three times。Table 4 it is shown that this porous material to cigarette smoke index without negative effect, wherein tar content and CO content decrease, and moisture has unexpected raising。
Table 4 composite filter tip Medicated cigarette conventional index detects
Embodiment 3
Residue after fragrant plant extraction described in the present embodiment, by raw material violet, lavandula angustifolia extracted after residual residue is filtered, microwave treatment 5min under the microwave power of 700W, then by the material after microwave treatment 70 DEG C of drying, screening after crushed obtains the powder of 60 orders。
The preparation method of residue porous material after fragrant plant of the present invention extraction, specifically include following steps: the ratio that the violet of 60 orders, Herba Lysimachiae foenum-graeci extract residue powder are 1:6 with mass ratio jointly put in tube furnace with KOH pressed powder, with the programming rate of 15 DEG C/min to 600 DEG C under argon atmosphere, insulation 20min, clean with the HCl that concentration is 15% subsequently and remove KOH, it is neutral for cleaning to pH value with distilled water, is finally dried to constant weight at 120 DEG C by material。
Select specific standard tow, porous material carrying out charge bar on KDF-2E forming machine roll, select specification tow to roll white rod on KDF-2E forming machine, charge bar carries out composite molding with white rod on composite molding machine, rolling into binary compound filter candle, recombination length is 1:1;This porous material addition in mouth rod is that 25mg/ props up。
Then Medicated cigarette sensory evaluating smoking is carried out by panel of expert of smokeing panel test by the regulation of " GB5606.4-1996 Medicated cigarette sense organ technology requirement "。Control sample is do not add the normal Medicated cigarette of porous material, and smoking result is in Table 3。Smoking result in table 3 shows, this porous material can make cigarette perfume (or spice) finer and smoother, reduces and stimulates, does not change original style and features of Medicated cigarette。
Table 3 Medicated cigarette sensory evaluating smoking's result
For analyzing this porous material absorption effect further, according to the relevant criterion of GB5606.5-2005, the main flume of Medicated cigarette being commonly performed analysis, result is in Table 4, and result is the meansigma methods after surveying three times。Table 4 it is shown that this porous material to cigarette smoke index without negative effect, wherein tar content and CO content decrease, and moisture has unexpected raising。
Table 4 composite filter tip Medicated cigarette conventional index detects
Embodiment 4
Residue porous material after fragrant plant extraction described in the present embodiment, by raw material Flos Chrysanthemi, Herba Convallariae, cloud Flos Carthami extracted after residual residue is filtered, microwave treatment 15min under the microwave power of 400W, then by the material after microwave treatment 80 DEG C of drying, screening after crushed obtains the powder of 40 orders。
The preparation method of residue porous material after fragrant plant of the present invention extraction, specifically include following steps: the ratio that the Flos Chrysanthemi of 40 orders, Herba Convallariae, cloud Flos Carthami extract residue powder are 1:5 with mass ratio jointly put in tube furnace with KOH pressed powder, with the programming rate of 10 DEG C/min to 650 DEG C under argon atmosphere, insulation 30min, clean with the HCl that concentration is 12% subsequently and remove KOH, it is neutral for cleaning to pH value with distilled water, is finally dried to constant weight at 130 DEG C by material。
Select specific standard tow, porous material carrying out charge bar on KDF-2E forming machine roll, select specification tow to roll white rod on KDF-2E forming machine, charge bar carries out composite molding with white rod on composite molding machine, rolling into binary compound filter candle, recombination length is 1:1;This porous material addition in mouth rod is that 30mg/ props up。
Then Medicated cigarette sensory evaluating smoking is carried out by panel of expert of smokeing panel test by the regulation of " GB5606.4-1996 Medicated cigarette sense organ technology requirement "。Control sample is do not add the normal Medicated cigarette of porous material, and smoking result is in Table 3。Smoking result in table 3 shows, this porous material can make cigarette perfume (or spice) finer and smoother, reduces and stimulates, does not change original style and features of Medicated cigarette。
Table 3 Medicated cigarette sensory evaluating smoking's result
For analyzing this porous material absorption effect further, according to the relevant criterion of GB5606.5-2005, the main flume of Medicated cigarette being commonly performed analysis, result is in Table 4, and result is the meansigma methods after surveying three times。Table 4 it is shown that this porous material to cigarette smoke index without negative effect, wherein tar content and CO content decrease, and moisture has unexpected raising。
Table 4 composite filter tip Medicated cigarette conventional index detects
Embodiment 5
Residue porous material after fragrant plant extraction described in the present embodiment, with Radix Inulae, Flos Chrysanthemi, Herba Convallariae, cloud Flos Carthami, Flos Rosae Rugosae extracted after residual residue is filtered, microwave treatment 9min under the microwave power of 660W, then by the material after microwave treatment 90 DEG C of drying, screening after crushed obtains the powder of 80 orders。
The preparation method of residue porous material after fragrant plant of the present invention extraction, specifically include following steps: the ratio that the Radix Inulae of 80 orders, Flos Chrysanthemi, Herba Convallariae, cloud Flos Carthami, rose extract residue powder are 1:4 with mass ratio jointly put in tube furnace with KOH pressed powder, with the programming rate of 10 DEG C/min to 600 DEG C under argon atmosphere, insulation 20min, clean with the HCl that concentration is 15% subsequently and remove KOH, it is neutral for cleaning to pH value with distilled water, is finally dried to constant weight at 150 DEG C by material。
Select specific standard tow, porous material carrying out charge bar on KDF-2E forming machine roll, select specification tow to roll white rod on KDF-2E forming machine, charge bar carries out composite molding with white rod on composite molding machine, rolling into binary compound filter candle, recombination length is 1:1;This porous material addition in mouth rod is that 20mg/ props up。
Then Medicated cigarette sensory evaluating smoking is carried out by panel of expert of smokeing panel test by the regulation of " GB5606.4-1996 Medicated cigarette sense organ technology requirement "。Control sample is do not add the normal Medicated cigarette of porous material, and smoking result is in Table 3。Smoking result in table 3 shows, this porous material can make cigarette perfume (or spice) finer and smoother, reduces and stimulates, does not change original style and features of Medicated cigarette。
Table 3 Medicated cigarette sensory evaluating smoking's result
For analyzing this porous material absorption effect further, according to the relevant criterion of GB5606.5-2005, the main flume of Medicated cigarette being commonly performed analysis, result is in Table 4, and result is the meansigma methods after surveying three times。Table 4 it is shown that this porous material to cigarette smoke index without negative effect, wherein tar content and CO content decrease, and moisture has unexpected raising。
Table 4 composite filter tip Medicated cigarette conventional index detects

Claims (5)

1. residue porous material after a fragrant plant extraction, it is characterised in that it is prepared by the method comprised the following steps:
(1) after being extracted by fragrant plant, residue carries out microwave treatment, the condition of described microwave treatment is microwave power 350~750W, microwave treatment time is 5~20min, then the fragrant plant after microwave treatment is taken rear residue and dries to constant weight at 70~110 DEG C;
(2) material obtained for step (1) is mixed with KOH pressed powder with the ratio that mass ratio is 1:2~1:6, with the programming rate of 5~20 DEG C/min to 500~700 DEG C in argon atmosphere, keep 10~30min at this temperature;
(3) HCl that material concentration is 5%~15% step (2) obtained cleans and removes KOH, then clean after being neutrality to pH value with distilled water, dry to constant weight at 100~150 DEG C, namely obtain residue porous material after described fragrant plant is extracted。
2. residue porous material after fragrant plant according to claim 1 extraction, it is characterised in that after wherein said fragrant plant is extracted, residue is fragrant plant residue after water extraction or alcohol extraction。
3. residue porous material after fragrant plant according to claim 2 extraction, it is characterized in that, wherein said fragrant plant selected from Flos Rosae Rugosae, Herba Menthae, Herba Rosmarini Officinalis, Flos Chrysanthemi, Herba Convallariae, cloud Flos Carthami, tree orchid, violet, lavandula angustifolia, one or more in Radix Inulae。
4. after fragrant plant according to claim 1 is extracted, residue porous material is used for mixing in cigarette filter with to cigarette smoke reducing tar and reducing harm and/or the purposes increasing flue gas moist feeling。
5. purposes according to claim 4, it is characterised in that after described fragrant plant is extracted, residue porous material incorporation in cigarette filter is that 15mg~30mg/ props up。
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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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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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 powdered 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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