CN103341347B - Adsorbent for selectively reducing release amount of volatile carbonyl and phenol compounds in cigarette smoke and preparation method and application of adsorbent - Google Patents
Adsorbent for selectively reducing release amount of volatile carbonyl and phenol compounds in cigarette smoke and preparation method and application of adsorbent Download PDFInfo
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Abstract
The invention discloses an adsorbent for selectively reducing the release amount of volatile carbonyl and phenol compounds in cigarette smoke and a preparation method and application of the adsorbent. The preparation method comprises the following steps of: preparing an aqueous solution of inorganic metal salt, directly spraying the aqueous solution on the surface of any one carrier material of activated carbon fibers, a zeolite molecular sieve, sepiolite, activated carbon and the like, performing drying treatment and preparing the adsorbent. When the adsorbent is applied to cigarettes in a binary composite filter stick form, the release amount of multiple volatile carbonyl compounds and phenol compounds in main stream smoke of the cigarettes can be greatly reduced while the sensory quality of the cigarettes is not obviously influenced. The adsorbent has the obvious effect of selectively reducing the cigarette harm, is extremely simple in preparation process, low in cost and safe, has the effect of environment protection, and has wide application prospects in the field of cigarette harm reduction, and the large-scale industrial production of the adsorbent is easily realized.
Description
Technical field
The present invention relates to the preparing technical field of Tar and cigarette filter, be specifically related to a kind of can the adsorbent and its preparation method and application of phenols and carbonyls burst size in selectivity reducing cigarette main flume.
Background technology
There is a series of chemistry, the physical changes such as pyrolysis, degraded, distillation in combustion in cigarette, the cigarette smoke complicated components formed, the composition having identified out is up to kind more than 5000, and volatile carbonyl and phenolic compound are wherein important harmful and carcinogenic components.There are some researches show that the volatile carbonyl compounds such as the formaldehyde of below five carbon, acetaldehyde, crotonaldehyde can be absorbed by suction, skin and cause disease, particularly crotonaldehyde is highly toxic substance, there is ciliary toxicity, after it is sucked by human body together with hydrogen cyanide, can PUD D be caused, can nervous system disorder be caused in addition.Several simple phenols component such as phenol, catechol may cause chromosome aberration and sister chromatid exchange, has certain genotoxicity and carcinogenicity, and catechol is classified as the carcinogenic substance suspicious to the mankind by international cancer research institution (IARC).In view of this, volatile carbonyl and phenolic compound are listed in the control ingredients list of suggestion by WHO " tobacco product control research group ", Her Majesty the Queen in right of Canada as represented by the minister of Healt is also listed in detects list (the Hoffmann list of correction), and requires its content of periodic detection in production of cigarettes and make public.
Along with the public is to the pay attention to day by day of smoking and health problem, reduce cigarette smoke harmful components burst size and there is very important realistic meaning, adopt transition metal or noble metal additive to prepare the study hotspot that Compound filtering material is also current tobacco science and technology with the harmful substance reduced in cigarette mainstream flue gas.World patent WO2005/013733 discloses and is added in pipe tobacco or cigarette wrapping paper by the catalyst such as platinum oxide or palladium oxide, at least can reduce the CO burst size of in flue gas 10%.The noble metal catalyst that world patent WO2007/096785 openly adopts the method such as deposition sedimentation, co-precipitation to synthesize, by 2wt.%Au-TiO
2(50 ~ 350mg 50 order size) catalyst adds in filter tip, can reduce by the CO of in main flume 10 ~ 50%.Chinese patent CN1921936A reduces the noble metal catalyst (containing gold, palladium and platinum) of CO content in cigarette smoke under disclosing a kind of normal temperature, can reduce the CO of in main flume 20 ~ 45%.
Patent WO99/11358 (1999) is by ion-exchange carried metal copper, cobalt on the activated carbon, the metal ions such as chromium and silver, have developed a kind of modified activated carbon absorbent, effectively can adsorb the harmful substances such as HCN, but " the carbon taste " in active carbon brings offending sensation to smoker.Patent CN141695A and CN1462652A etc. have set forth catalytic oxidation reducing the effect in cigarette in hydrogen cyanide, show higher catalytic activity.But production cost is higher, and in process of production, have the skewness phenomenon in single cigarette, restive.The patent document of Microamounts of Hydrogen cyanic acid in catalytic oxidation and absorption method filtering cigarette mainstream flue gas is adopted also to have report.The catalytic temperature of catalytic oxidation higher (as patent CN1462652A, catalytic temperature requires 250-450 DEG C), required catalyst is expensive, production cost high (as patent CN1583257A adopts nm of gold, and complex manufacturing process).US4091822 utilizes amine and the Zn of many dentates
2+, Fe
2+and Cu
2+after complexing of metal ion, be combined with polyalkylene oxide and form adsorbent and remove HCN in cigarette smoke.Chinese patent 201010542254.8 utilizes CN-and metal ion to have this feature of stronger complexing, metal ions different in complexing on the porous carrier of bigger serface, obtain the HCN burst size that a metalloid complex materials can be used in selectivity reducing cigarette fume, but the flow process of preparation complex materials is more, complex procedures, also need at the metal ion of supported on carriers more than three kinds or three kinds.
Adopt the patent of metal ion or metal oxide reduction phenolic compounds in cigarette smoke or carbonyls, document still rare.Chinese patent CN101116540A discloses one " tobacco additive agent and its preparation method and application for reducing content of group compounds of aldehydes and ketones in cigarette smoke ", CN102697179A the present invention is with the compound of one or more amino acid and transition metal salt for active component prepares compound material, and in flue gas, the range of decrease of formaldehyde, acetaldehyde and crotonaldehyde is about 30%.CN101194756A utilizes shitosan and metal ion to prepare chitosan complex, and the aldehyde material in flue gas reduces 27.1%.CN102228311A discloses a kind of adsorbent with phenol in selectivity reducing cigarette main flume, and this adsorbent passes through at SiO
2middle doped with Al
2o
3, MgO/CaO, CuO porous oxide composite, prepare through multi-step process.Chinese patent CN1692848A discloses a kind of modified active carbon fiber of removing the evil for tobacco smoke filter element and preparation method thereof (TiO
2-Pd-Cu based active carbon fiber), modified active carbon fiber and acetate fiber are made cigarette composite filter tip, the content of CO and fatty aldehyde material in cigarette smoke can be reduced.It is more to there is preparation section in these patented technologies, complex process, or active component exists the problems such as certain security, and the amino acid cost that some patents use is higher, and these problems all limit scale, the industrialized mass production of these patented technologies.
In summary, the research adopting at present metal or metal oxide to reduce cigarette mainstream flue gas harmful components mainly concentrates on composition burst size fields such as reducing in flue gas CO, HCN, unique nitrosamine.Adopt a kind of metal ion adsorbent, do not affecting the sucking quality of cigarette, under ensureing that cigarette smoke does not introduce the prerequisite of new unsafe factor, can the simultaneously selective burst size significantly reducing multiple volatile carbonyl compound and aldehydes matter in cigarette mainstream flue gas, but also have preparation technology simple, can produce in batches, the technology possessing application prospect is fallen burnt field at Harm reduction techniques and be there is not yet Patents and bibliographical information.
Summary of the invention
First technical problem that the present invention will solve is to provide the preparation method of the adsorbent of volatile carbonyl and phenolic compound burst size in a kind of selectivity reducing cigarette fume, and the method preparation process is simple, is easy to industrial applications and batch production.
Second technical problem that the present invention will solve is to provide the adsorbent of volatile carbonyl and phenolic compound burst size in a kind of selectivity reducing cigarette fume.
The 3rd technical problem that the present invention will solve is to provide the application of the adsorbent of volatile carbonyl and phenolic compound burst size in a kind of selectivity reducing cigarette fume.
For solving above-mentioned first technical problem, the preparation method of the adsorbent of volatile carbonyl and phenolic compound burst size in a kind of selectivity reducing cigarette fume of the present invention, comprises the following steps:
1) inorganic metal salt is water-soluble, the aqueous solution of preparation inorganic metal salt;
2) aqueous solution of inorganic metal salt step 1) prepared evenly is sprayed on carrier material and obtains the composite that load has metal ion, and the metal ion quality of load is 10 ~ 40% of carrier material quality;
3) by step 2) composite that obtains carries out drying and processing 30 ~ 60min under being placed in 100 ~ 150 DEG C of conditions, obtains adsorbent of the present invention.
Further, the aqueous solution of inorganic metal salt described in step 1) is copper chloride (CuCl
2), stannous chloride (CuCl), copper sulphate (CuSO
4), nickel chloride (NiCl
2) or nickelous sulfate (NiSO
4) the aqueous solution in any one or wherein any one and palladium bichloride (PdCl
2) the mixture of the aqueous solution.
Further, described in step 1), the mass percent concentration of inorganic metal saline solution is 5 ~ 30%.
Further, described copper chloride (CuCl
2), stannous chloride (CuCl), copper sulphate (CuSO
4), nickel chloride (NiCl
2) or nickelous sulfate (NiSO
4) the aqueous solution and palladium bichloride (PdCl
2) the composite volume ratio of the aqueous solution be 1:1 ~ 5:1.
Further, described carrier material comprises any one in NACF, zeolite molecular sieve, sepiolite or active carbon.
For solving above-mentioned second technical problem, the present invention prepares the adsorbent of volatile carbonyl and phenolic compound burst size in selectivity reducing cigarette fume by said method.Described adsorbent is not affecting in cigarette while aesthetic quality, and efficient selective reduces the burst size of multiple volatile carbonyl compound and aldehydes matter in cigarette mainstream flue gas, reduces smoking to the harm of human body.
For solving above-mentioned 3rd technical problem, the application of adsorbent of the present invention volatile carbonyl and phenolic compound burst size in selectivity reducing cigarette fume, described adsorbent uses as the additive of cigarette filter stick of volatile carbonyl compound and aldehydes matter burst size in selectivity reducing cigarette main flume.
Further, described adsorbent and cellulose acetate filter rod make binary compound filter candle or coaxial core binary compound filter candle, often prop up in filter stick containing adsorbent 3 ~ 15mg.
The present invention has following beneficial effect:
When adsorbent prepared by preparation method of the present invention is for cigarette filter rod, the tar content fall of cigarette is less, but significantly can reduce the burst size of multiple volatile carbonyl compound and aldehydes matter in cigarette mainstream flue gas simultaneously, for the crotonaldehyde that toxicity is larger, phenol and catechol, selectively lower efficiency respectively 31.7 ~ 50.8%, more than 35.3 ~ 45.6% and 37.7 ~ 48.2%, CO simultaneously in main flume and the content of hydrogen cyanide also all decrease, and harmful effect is not had to the sucking quality of cigarette, aesthetic quality does not have significant change, reach the object of selectivity reducing cigarette harmfulness.
The present invention, compared with the technology such as existing metal complex, complex materials, also has following advantage:
1) security of the present invention is higher, and the inorganic metal salt of employing is material cheap and easy to get, does not adopt all the other auxiliary materials, meets food safety and sanitation requirement, does not introduce new unsafe factor to cigarette smoke.
2) in the present invention, inorganic metal salt is mixed with the aqueous solution, can directly use after being evenly sprayed on carrier material, oven dry, and preparation process is extremely simple, under existing process conditions, easily realizes industrialization, large-scale production.
3) the present invention is without steps such as any pickling, alkali cleanings, and in preparation process, do not use any organic solvent, whole process is discharged without waste water,waste gas and industrial residue, can not to environment.
4) manufacture craft of filter tip is the existing mature technology of industry, and therefore present invention process is simple, and it is very convenient to operate, with low cost during large-scale production.
Detailed description of the invention
Embodiment 1
1, the preparation of adsorbent
1) prepare mass fraction be 20% CuCl solution and mass fraction be the PdCl of 10%
2solution, the two obtains the mixed solution of the two with the volume mixture of 2:1;
2) mixed solution adopting sprayer step 1) to be prepared evenly is sprayed on NACF surface, and obtain the composite that load has metal ion Cu, Pd, wherein the load capacity of Cu, Pd element is respectively 21.4% and 12.5% of NACF quality;
3) by step 2) composite that obtains in 120 DEG C of drying and processing 40min, obtain adsorbent of the present invention.
2, the application of adsorbent
Adopt the existing forming method of filter stick for cigarettes and cellulose acetate filter rod to make coaxial core binary combined filter tip the sorbent material of preparation, trial-production quantity is 0.8 ten thousand, and often propping up the sorbent material contained in cigarette is 6mg.
3, comparative example
Cigarette used is not to add the material modified cigarette of any filter tip for control sample.
4, detect
Before cigarette test used under temperature (22 ± 1) DEG C, relative humidity (60 ± 2) % condition balance 48 hours.
On smoking machine, cigarette smoking test is carried out according to standard aspiration condition, and according to the YC/T255-2008 " the mensuration high performance liquid chromatography of main phenolic compounds in main stream smoke of cigarette " of standard tobacco industry, YC/T254-2008 " the mensuration high performance liquid chromatography of main carbonyl compounds in main stream cigarette smoke ", the GB/T23356-2009 mensuration non-scatter infrared method of carbon monoxide " in the cigarette smoke in gas phase ", the YC/T253-2008 mensuration continuous flow method of hydrogen cyanide " in the cigarette mainstream flue gas " phenolic compound in smoke, carbonyls, the detection of CO and hydrocyanic acid release amount and releasing content of coke tar, measurement result is in table 1.
Result shows, after adsorbent is applied to cigarette, can significantly major phenolic compound and volatile carbonyls in selective reduction main flume, and the CO simultaneously in flue gas and the content of hydrogen cyanide also decrease.The cigarette adopting product of the present invention to prepare is smoked panel test after the judging panel of qualification smokes panel test think through being had industry, and compared with contrast cigarette, the aesthetic quality of cigarette does not change substantially.Cigarette mainstream flue gas shows through icp ms measurement result, in the main flume of use sorbent material, Cu element and the content of Pd element are compared with contrast cigarette, there is no significant difference, show that invention product meets the safety indexes requirement of food.
Embodiment 2
1, the preparation of adsorbent
Preparation mass fraction is the CuCl of 30%
2solution, adopts sprayer by CuCl
2dissolution homogeneity is sprayed on NACF surface, and obtain the composite that load has metal ion Cu, wherein the load capacity of Cu element is respectively 13.6% of NACF quality; Then by composite in 120 DEG C of drying and processing 40min, obtain adsorbent of the present invention.
2, the application of adsorbent
Adopt the existing forming method of filter stick for cigarettes and cellulose acetate filter rod to make coaxial core binary combined filter tip the sorbent material of preparation, trial-production quantity is 0.8 ten thousand, and often propping up the sorbent material contained in cigarette is 15mg.
All the other steps are with embodiment 1, and measurement result is in table 1.
Result shows, after adsorbent is applied to cigarette, can significantly major phenolic compound and volatile carbonyls in selective reduction main flume, and the CO simultaneously in flue gas and the content of hydrogen cyanide also decrease.The cigarette adopting product of the present invention to prepare is smoked panel test after the judging panel of qualification smokes panel test think through being had industry, and compared with contrast cigarette, the aesthetic quality of cigarette does not change substantially.Cigarette mainstream flue gas shows through icp ms measurement result, uses the content of Cu element in the main flume of sorbent material compared with contrast cigarette, does not have significant difference, show that invention product meets the safety indexes requirement of food.
Embodiment 3
Preparation mass fraction is the NiCl of 20%
2solution, adopt sprayer be evenly sprayed on zeolite molecular sieve surface, the load capacity of Ni element is 30% of zeolite molecular sieve quality, then by composite in 150 DEG C of drying and processing 40min.The sorbent material of preparation adopts the existing forming method of filter stick for cigarettes and cellulose acetate filter rod to make binary combined filter tip, and trial-production quantity is 0.8 ten thousand, and often propping up the sorbent material contained in cigarette is 11mg.All the other steps are with embodiment 1, and measurement result is in table 1.
Result shows, after adsorbent is applied to cigarette, can significantly major phenolic compound and volatile carbonyls in selective reduction main flume, and the CO simultaneously in flue gas and the content of hydrogen cyanide also decrease.The cigarette adopting product of the present invention to prepare is smoked panel test after the judging panel of qualification smokes panel test think through being had industry, and compared with contrast cigarette, the aesthetic quality of cigarette does not change substantially.Cigarette mainstream flue gas shows through icp ms measurement result, uses the content of Ni element in the main flume of sorbent material compared with contrast cigarette, does not have significant difference, show that invention product meets the safety indexes requirement of food.
Embodiment 4
Preparation mass fraction is the NiSO of 30%
4solution, adopt sprayer be evenly sprayed on sepiolite surface, the load capacity of Ni element is 25% of sepiolite quality, then by composite in 150 DEG C of drying and processing 40min.The sorbent material of preparation adopts the existing forming method of filter stick for cigarettes and cellulose acetate filter rod to make binary combined filter tip, and trial-production quantity is 0.8 ten thousand, and often propping up the sorbent material contained in cigarette is 15mg.All the other steps are with embodiment 1, and measurement result is in table 1.
Result shows, after adsorbent is applied to cigarette, can significantly major phenolic compound and volatile carbonyls in selective reduction main flume, and the CO simultaneously in flue gas and the content of hydrogen cyanide also decrease.The cigarette adopting product of the present invention to prepare is smoked panel test after the judging panel of qualification smokes panel test think through being had industry, and compared with contrast cigarette, the aesthetic quality of cigarette does not change substantially.Cigarette mainstream flue gas shows through icp ms measurement result, uses the content of Ni element in the main flume of sorbent material compared with contrast cigarette, does not have significant difference, show that invention product meets the safety indexes requirement of food.
Embodiment 5
Preparation mass fraction be 40% NiCl2 solution and mass fraction be the PdCl of 15%
2solution, the two is evenly sprayed on NACF surface to adopt sprayer after the volume mixture of 5:1, and the load capacity of Ni, Pd element is respectively 40% and 20% of NACF quality, then by composite in 120 DEG C of drying and processing 40min.The sorbent material of preparation adopts the existing forming method of filter stick for cigarettes and cellulose acetate filter rod to make coaxial core binary combined filter tip, and trial-production quantity is 0.8 ten thousand, and often propping up the sorbent material contained in cigarette is 15mg.All the other steps are with embodiment 1, and measurement result is in table 1.
Result shows, after adsorbent is applied to cigarette, can significantly major phenolic compound and volatile carbonyls in selective reduction main flume, and the CO simultaneously in flue gas and the content of hydrogen cyanide also decrease.The cigarette adopting product of the present invention to prepare is smoked panel test after the judging panel of qualification smokes panel test think through being had industry, and compared with contrast cigarette, the aesthetic quality of cigarette does not change substantially.Cigarette mainstream flue gas shows through icp ms measurement result, use the content of Ni element and Pd element in the main flume of sorbent material compared with contrast cigarette, there is no significant difference, show that invention product meets the safety indexes requirement of food.
Embodiment 6
Preparation mass fraction is the CuSO of 40%
4solution, adopt sprayer be evenly sprayed on activated carbon surface, the load capacity of Cu element is 10% of quality of activated carbon, then by composite in 150 DEG C of drying and processing 40min.The sorbent material of preparation adopts the existing forming method of filter stick for cigarettes and cellulose acetate filter rod to make binary combined filter tip, and trial-production quantity is 0.8 ten thousand, and often propping up the sorbent material contained in cigarette is 15mg.All the other steps are with embodiment 1, and measurement result is in table 1.
Result shows, after adsorbent is applied to cigarette, can significantly major phenolic compound and volatile carbonyls in selective reduction main flume, and the CO simultaneously in flue gas and the content of hydrogen cyanide also decrease.The cigarette adopting product of the present invention to prepare is smoked panel test after the judging panel of qualification smokes panel test think through being had industry, and compared with contrast cigarette, the aesthetic quality of cigarette does not change substantially.Cigarette mainstream flue gas shows through icp ms measurement result, uses the content of Cu element in the main flume of sorbent material compared with contrast cigarette, does not have significant difference, show that invention product meets the safety indexes requirement of food.
What the composite filter tip of embodiment 1 ~ 6 made that main flume releasing content of coke tar in cigarette and harmful components reduce amplitude the results are shown in Table 1.
Table 1 cigarette sample tar content and each harmful components burst size and the amplitude of reduction
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (5)
1. the preparation method of the adsorbent of volatile carbonyl and phenolic compound burst size in selectivity reducing cigarette fume, is characterized in that, be made up of following steps:
1) inorganic metal salt is water-soluble, the aqueous solution of preparation inorganic metal salt;
2) by step 1) aqueous solution of inorganic metal salt prepared evenly is sprayed on carrier material and obtains the composite that load has metal ion, and the metal ion quality of load is 10 ~ 40% of carrier material quality;
3) by step 2) composite that obtains carries out drying and processing 30 ~ 60min under being placed in 100 ~ 150 DEG C of conditions, obtains adsorbent;
Step 1) aqueous solution of described inorganic metal salt is any one in the aqueous solution of copper chloride, stannous chloride, copper sulphate, nickel chloride or nickelous sulfate;
Step 2) described carrier material is selected from any one in NACF or sepiolite.
2. the preparation method of the adsorbent of volatile carbonyl and phenolic compound burst size in selectivity reducing cigarette fume according to claim 1, is characterized in that, step 1) mass percent concentration of described inorganic metal saline solution is 5 ~ 30%.
3. the adsorbent of volatile carbonyl and phenolic compound burst size in the selectivity reducing cigarette fume that method obtains as described in any one of claim 1-2.
4. the application of the adsorbent of volatile carbonyl and phenolic compound burst size in selectivity reducing cigarette fume according to claim 3, it is characterized in that, described adsorbent uses as the additive of cigarette filter stick of volatile carbonyl compound and aldehydes matter burst size in selectivity reducing cigarette main flume.
5. the application of the adsorbent of volatile carbonyl and phenolic compound burst size in selectivity reducing cigarette fume according to claim 4, it is characterized in that, described adsorbent and cellulose acetate filter rod make binary compound filter candle or coaxial core binary compound filter candle, often prop up in filter stick containing adsorbent 3 ~ 15mg.
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| CN103785272A (en) * | 2014-01-29 | 2014-05-14 | 北京创联伍杰科技有限公司 | Extraction device and extraction method for tobacco bois flavors in tobacco processing waste gas |
| CN107185584B (en) * | 2017-05-05 | 2020-06-16 | 北京华福工程有限公司 | Catalyst for synthesizing acrylic acid low-carbon alcohol ester from acetylene and preparation method and application thereof |
| CN107688064B (en) * | 2017-08-30 | 2020-07-03 | 国家烟草质量监督检验中心 | Method for simultaneously detecting carbonyl compound and phenolic compound in main stream smoke of cigarette |
| CN108835709B (en) * | 2018-03-21 | 2020-10-27 | 云南中烟工业有限责任公司 | Modified molecular sieve additive for reducing CO release amount in smoke and preparation method and application thereof |
| CN112167706B (en) * | 2020-09-28 | 2022-09-02 | 江苏中烟工业有限责任公司 | Additive for cigarette filter stick for reducing ammonia in cigarette smoke and preparation method and application thereof |
| CN112108105B (en) * | 2020-10-19 | 2023-01-31 | 江苏中烟工业有限责任公司 | Adsorbing material for reducing HCN and phenol in cigarette smoke and application thereof |
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| CN2803014Y (en) * | 2005-04-14 | 2006-08-09 | 南京师范大学 | Copper-palladium base modified active carbon fiber compounded filter-tip of cigarrete |
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