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CN108158034A - A kind of preparation method of composite aerogel type cigarette filter tip materials - Google Patents

A kind of preparation method of composite aerogel type cigarette filter tip materials Download PDF

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Publication number
CN108158034A
CN108158034A CN201711278092.XA CN201711278092A CN108158034A CN 108158034 A CN108158034 A CN 108158034A CN 201711278092 A CN201711278092 A CN 201711278092A CN 108158034 A CN108158034 A CN 108158034A
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China
Prior art keywords
temperature
filter tip
cigarette filter
composite aerogel
type cigarette
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CN201711278092.XA
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Inventor
张琳
许玉
陈水
陈一水
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Changzhou Jie Xuan Textile Technology Co Ltd
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Changzhou Jie Xuan Textile Technology Co Ltd
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Priority to CN201711278092.XA priority Critical patent/CN108158034A/en
Publication of CN108158034A publication Critical patent/CN108158034A/en
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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
    • A24D3/02Manufacture of tobacco smoke filters
    • 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
    • A24D3/067Use of materials for tobacco smoke filters characterised by functional properties

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Seasonings (AREA)

Abstract

The invention discloses a kind of preparation methods of composite aerogel type cigarette filter tip materials, belong to filtering material preparing technical field.Ultrasonic immersing after the present invention first mixes sepiolite with organic acid soln, again through being concentrated under reduced pressure, drying, roasting, sepiolite must be pre-processed, pretreatment sepiolite is reacted with organic base again, it is concentrated under reduced pressure, dry modified meerschaum, then carbomer, phosphatide and carragheen are added to the water, after ultrasonic disperse, glycoprotein is added, constant temperature is stirred to react, and obtains mixed liquor, it again will be in injection mold after modified meerschaum and the stirring of mixed liquor constant temperature, the vacuum freeze drying after low temperature is pre-chilled is demoulded to get composite aerogel type cigarette filter tip materials.Composite aerogel type cigarette filter tip materials prepared by technical solution of the present invention have excellent absorption property, to the adsorption effect outstanding feature of harmful substance in cigarette, and with preferable mechanical property, and can retain the fragrance of cigarette.

Description

A kind of preparation method of composite aerogel type cigarette filter tip materials
Technical field
The invention discloses a kind of preparation methods of composite aerogel type cigarette filter tip materials, belong to filtering material preparation Technical field.
Background technology
Cigarette filter initial design is that cigarette paper sticks on lip and prevent pipe tobacco from sucking oral cavity when aspirating in order to prevent. But after researcher issues in relation to the epidemiological study result that Smoking is harmful to your health, consumer's Dichlorodiphenyl Acetate fibrous filter end The accreditation of face appearance and tar reduction effect causes the cellulose acetate filter market share to steeply rise, and filter tip becomes the indispensable portion of cigarette Point.As society is to the growing interest smoked with health problem, tobacco business scientific research personnel is in filter material modification and exploitation, filter tip ginseng Numerous studies, the filter tip reducing tar and reducing harm skill of exploitation are carried out in the fields such as number optimization, filter structures design and additives of filter tip technology Art significantly reduces tarry matters in smoke, harmful components burst size, wherein filter tip Parameters Optimal Design, groove filter tip technology, activity Charcoal particle filter tip technology, ventilation filter tip technology etc. are applied increasingly extensively, and in reducing tar and reducing harm and show cigarette on cigarette product Play an important roll on Brand characteristic.At present, the filter tip retention efficiency in relation to the flue gases conventional ingredient such as cigarette smoke nicotine, tar Research more have been reported that, but main harmful components, especially tobacco-specific nitrosamine in related flue gas(TSNAs)Filter tip retention effect The rare report of research of rate.The pathogenesis of TSNAs is tentatively illustrated in recent years.But some critical problems according to So failing to solve, the formation mechenism of TSNAs not yet thoroughly illustrates, and to the technology of nitrosamine in flue gas of how degrading, though have one It is a little to break through, at present still without well solving.At present, to reduce TSNAs using physical technique more.Conventional method is by rolling up It is metal oxide-loaded that 2%~5% is added in cigarette pipe tobacco(The oxide of magnesium, zinc, iron, manganese etc.)Zeolite, to reduce mainstream and side Flow the nitrosamine total amount in flue gas.Sub- wait is worn to extract a variety of ketone, phenols and its derivative from pteridophyte natural plants and obtain Compound additive is made an addition to 0.008% ratio in cigarette filter or pipe tobacco, a variety of condensed-nuclei aromatics in main flume, from Also there is reduction by the carcinogenic content such as base and aromatic amine, also have certain scavenging effect to TSNAs in flue gas, but remove effect Fruit is still barely satisfactory.
Therefore, the shortcomings that how improving conventional cigarette filter-tip material absorption property and bad mechanical property, to obtain more The cigarette filter tip materials of high combination property are that it is promoted and applies, meet industrial production demand urgent problem to be solved.
Invention content
The present invention solves the technical problem of:For conventional cigarette filter-tip material absorption property and mechanical property not The shortcomings that good, provides a kind of preparation method of composite aerogel type cigarette filter tip materials.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)It is 1 in mass ratio by sepiolite and organic acid soln:10~1:After 20 mixing, ultrasonic immersing, then through being concentrated under reduced pressure, Dry, roasting obtains pretreatment sepiolite;
(2)It is 1 in mass ratio that sepiolite, which will be pre-processed, with organic alkali solution:10~1:After 15 mixing, constant temperature is stirred to react, then is passed through It is concentrated under reduced pressure, it is dry, obtain modified meerschaum;
(3)It counts in parts by weight, takes 30~40 parts of carbomers, 8~10 parts of glycoprotein, 6~8 parts of phosphatide, 4~6 parts of OK a karaoke clubs successively Carbomer, phosphatide and carragheen, are first added to the water by glue, 200~300 parts of water, after ultrasonic disperse, add glycoprotein, constant temperature It is stirred to react, obtains mixed liquor;
(4)It is 1 in mass ratio:8~1:After 10 are stirred modified meerschaum and mixed liquor constant temperature, inject in mold, then pass through After low temperature precooling, vacuum freeze drying is demoulded to get composite aerogel type cigarette filter tip materials.
Step(1)It is 3 in mass ratio by oxalic acid, citric acid and water that the organic acid soln, which is,:1:20 are configured.
Step(2)The organic alkali solution is the tetrapropylammonium hydroxide solution that mass fraction is 10~15%.
Step(3)The carbomer is carbomer 910, any one in carbomer 934 or Acritamer 940.
Step(3)The glycoprotein is any one in Swine serum mucoprotein, cow's serum mucoprotein or chicken serum mucoprotein Kind.
Step(3)The phosphatide is any one in soybean lecithin or egg lecithin.
Step(4)The low temperature is pre-chilled:Under the conditions of temperature is -30~-28 DEG C, 6~8h is pre-chilled.
The beneficial effects of the invention are as follows:
(1)Technical solution of the present invention is by preparing a kind of filter-tip material of aerogel type, wherein containing having excellent adsorptivity The active ingredients such as sepiolite, carbomer, glycoprotein, the carragheen of energy, in preparation process, first, utilize organic acid and Hai Pao Stone carries out ultrasonic immersing, and hydrogen ion in acid solution is made to replace magnesium ion in sepiolite skeleton, connects sepiolite crystals channel It is logical, sepiolite specific surface area is made effectively to be promoted, and coordinate roasting, organic acid, which decomposes, in roasting process, in hole generates gas, can Sepiolite pore structure is further enriched, so as to improve its absorption property, tetrapropylammonium hydroxide is recycled to carry out sepiolite It is modified, make sepiolite skeleton structure that part desiliconization occur, non-skeleton silicon migration in system is made to be tied again to surface, and on surface Crystalline substance enables system internal gutter to dredge, and activated centre is exposed, and surface is regular, in addition, cooperation concentration and drying, make Organic base is deposited in sepiolite skeleton structure, and during being stirred to react with carbomer, organic base can be with carboxylic acid in carbomer Group combines, and makes to form gel inside system, and the use of carbomer can be with saccharide residue on glycoprotein oligonucleotide chain in system Hydrogen bond is formed, stronger mucous gels network is formed, so as to improve the mechanical property of gel rubber system and absorption property;
(2)The organic base used in technical solution of the present invention can decompose, after decomposition under flue gas heat effect in use Reactivate acidic-group active in carbomer, so as to largely adsorb the harmful substances such as tar, nitrosamine in flue gas, separately Outside, the salt fog that result of combustion of tobacco generates is made of a large amount of microlayer models, it often exists with suspension gaseous state, and the bands such as phosphatide, glycoprotein There is the addition of the substance of positive and negative charge, suspension gas particles can be made to reunite, and fixed and adsorb by system, and the technology of the present invention Each component retains the fragrance of cigarette with the use of alternative absorption harmful substances from flue gases in scheme.
Specific embodiment
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 20~ 30min obtains organic acid soln;After sepiolite ball milling, 300~500 mesh sieve is crossed, and the sepiolite after sieving and organic acid is molten Liquid is 1 in mass ratio:10~1:20 mixing after, in supersonic frequency be 45~55kHz, temperature be 45~55 DEG C under the conditions of, ultrasound Impregnate 1~3h, obtain maceration extract, and gained maceration extract is moved into Rotary Evaporators, in temperature be 65~75 DEG C, pressure for 500~ Under the conditions of 600kPa, 3~5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by No. 1 concentrate of gained in temperature be 85~95 DEG C of conditions Under, after dry 2~4h, tube furnace is transferred to, under the conditions of temperature is 350~400 DEG C, heat preservation 45~60min of roasting, furnace cooling To room temperature, discharging obtains pretreatment sepiolite;It is 1 in mass ratio that sepiolite and organic alkali solution, which will then be pre-processed,:10~1:15 It is 45~55 DEG C in temperature after mixing, under the conditions of rotating speed is 400~600r/min, constant temperature is stirred to react 2~4h, obtains reaction solution, And gained reaction solution is moved into Rotary Evaporators, it is 75~85 DEG C in temperature, under the conditions of pressure is 600~700kPa, decompression is dense Contract 3~5h, obtains No. 2 concentrates, and by No. 2 concentrates of gained be 85~90 DEG C in temperature under the conditions of dry 2~4h, sea must be modified Afrodite;It counts in parts by weight, takes 30~40 parts of carbomers successively, 8~10 parts of glycoprotein, 6~8 parts of phosphatide, 4~6 parts of carragheens, 200~300 parts of water, first pour into carbomer, phosphatide, carragheen and water in reaction kettle, in temperature be 65~75 DEG C, supersonic frequency Under the conditions of 45~55kHz, after 2~4h of ultrasonic disperse, then glycoprotein is added in into reaction kettle, be 75~85 with after temperature DEG C, under the conditions of rotating speed is 600~800r/min, constant temperature is stirred to react 3~5h, obtains mixed liquor;It is 1 in mass ratio:8~1:10 will Modified meerschaum and mixed liquor are poured into batch mixer, in rotating speed be 800~1200r/min, it is permanent under the conditions of temperature is 65~75 DEG C After temperature is stirred 4~6h, material in batch mixer is injected by syringe in mold, and mold is moved into refrigerator, Yu Wen Spend be -30~-28 DEG C under the conditions of be pre-chilled 6~8h, then by after precooling mold move into vacuum freezing drying oven, in temperature be -50 ~-48 DEG C, under the conditions of pressure is 20~30Pa, 24~36h of vacuum freeze drying, discharging is demoulded to get composite aerogel type perfume Tobacco filters material.The organic alkali solution is the tetrapropylammonium hydroxide solution that mass fraction is 10~15%.The carbomer Any one for carbomer 910, in carbomer 934 or Acritamer 940.The glycoprotein is Swine serum mucoprotein, cow's serum Any one in mucoprotein or chicken serum mucoprotein.The phosphatide is any one in soybean lecithin or egg lecithin Kind.
Example 1
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;After sepiolite ball milling, 500 mesh sieve is crossed, and is 1 in mass ratio by the sepiolite after sieving and organic acid soln:20 It is 55kHz in supersonic frequency after mixing, under the conditions of temperature is 55 DEG C, ultrasonic immersing 3h obtains maceration extract, and by gained maceration extract Rotary Evaporators are moved into, is 75 DEG C in temperature, under the conditions of pressure is 600kPa, 5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by institute No. 1 concentrate is obtained under the conditions of temperature is 95 DEG C, after dry 4h, is transferred to tube furnace, under the conditions of temperature is 400 DEG C, heat preservation roasts 60min is burnt, cools to room temperature with the furnace, discharges, obtains pretreatment sepiolite;Sepiolite then will be pre-processed and organic alkali solution presses matter Amount is than being 1:It is 55 DEG C in temperature after 15 mixing, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains reaction solution, and By gained reaction solution move into Rotary Evaporators, in temperature be 85 DEG C, pressure be 700kPa under the conditions of, be concentrated under reduced pressure 5h, obtain No. 2 it is dense Contracting liquid, and be 4h dry under the conditions of 90 DEG C in temperature by No. 2 concentrates of gained, obtain modified meerschaum;It counts in parts by weight, successively Take 40 parts of carbomers, 10 parts of glycoprotein, 8 parts of phosphatide, 6 parts of carragheens, 300 parts of water, first by carbomer, phosphatide, carragheen and water It pours into reaction kettle, is 75 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 4h, then is added in into reaction kettle Glycoprotein, with being 85 DEG C after temperature, under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 5h, obtains mixed liquor;In mass ratio It is 1:10 pour into modified meerschaum and mixed liquor in batch mixer, in rotating speed be 1200r/min, it is permanent under the conditions of temperature is 75 DEG C After temperature is stirred 6h, material in batch mixer is injected by syringe in mold, and mold is moved into refrigerator, in temperature 8h is pre-chilled under the conditions of being -28 DEG C, then the mold after precooling is moved into vacuum freezing drying oven, is -48 DEG C in temperature, pressure is Under the conditions of 30Pa, vacuum freeze drying 36h, discharging is demoulded to get composite aerogel type cigarette filter tip materials.It is described organic Aqueous slkali is the tetrapropylammonium hydroxide solution that mass fraction is 15%.The carbomer is carbomer 910.The glycoprotein is Swine serum mucoprotein.The phosphatide is soybean lecithin.
Example 2
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;It will count in parts by weight, and take 40 parts of carbomers successively, 10 parts of glycoprotein, 8 parts of phosphatide, 6 parts of carragheens, 300 parts of water, First carbomer, phosphatide, carragheen and water are poured into reaction kettle, is 75 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, surpasses After sound dispersion 4h, then glycoprotein is added in into reaction kettle, with being 85 DEG C after temperature, under the conditions of rotating speed is 800r/min, constant temperature 5h is stirred to react, obtains mixed liquor;It is 1 in mass ratio:10 pour into modified meerschaum and mixed liquor in batch mixer, are in rotating speed Material in batch mixer under the conditions of temperature is 75 DEG C, after constant temperature is stirred 6h, is injected mold by 1200r/min by syringe In, and mold is moved into refrigerator, 8h is pre-chilled under the conditions of being -28 DEG C in temperature, then the mold after precooling is moved into vacuum refrigeration Drying box is -48 DEG C in temperature, and under the conditions of pressure is 30Pa, vacuum freeze drying 36h, discharging is demoulded to get compound airsetting Glue-type cigarette filter tip materials.The organic alkali solution is the tetrapropylammonium hydroxide solution that mass fraction is 15%.The card wave Nurse is carbomer 910.The glycoprotein is Swine serum mucoprotein.The phosphatide is soybean lecithin.
Example 3
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;After sepiolite ball milling, 500 mesh sieve is crossed, and is 1 in mass ratio by the sepiolite after sieving and organic acid soln:20 It is 55kHz in supersonic frequency after mixing, under the conditions of temperature is 55 DEG C, ultrasonic immersing 3h obtains maceration extract, and by gained maceration extract Rotary Evaporators are moved into, is 75 DEG C in temperature, under the conditions of pressure is 600kPa, 5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by institute No. 1 concentrate is obtained under the conditions of temperature is 95 DEG C, after dry 4h, is transferred to tube furnace, under the conditions of temperature is 400 DEG C, heat preservation roasts 60min is burnt, cools to room temperature with the furnace, discharges, obtains pretreatment sepiolite;It counts in parts by weight, takes 40 parts of carbomers successively, 10 parts Glycoprotein, 8 parts of phosphatide, 6 parts of carragheens, 300 parts of water first pour into carbomer, phosphatide, carragheen and water in reaction kettle, Yu Wen It is 75 DEG C to spend, and under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 4h, then glycoprotein is added in into reaction kettle, with after temperature It it is 85 DEG C, under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 5h, obtains mixed liquor;It is 1 in mass ratio:10 will change pretreatment Sepiolite and mixed liquor are poured into batch mixer, are 1200r/min in rotating speed, under the conditions of temperature is 75 DEG C, constant temperature is stirred 6h Afterwards, material in batch mixer is injected by syringe in mold, and mold is moved into refrigerator, under the conditions of temperature is -28 DEG C Be pre-chilled 8h, then by after precooling mold move into vacuum freezing drying oven, in temperature be -48 DEG C, pressure be 30Pa under the conditions of, vacuum 36h is freeze-dried, discharging is demoulded to get composite aerogel type cigarette filter tip materials.The organic alkali solution is mass fraction For 15% tetrapropylammonium hydroxide solution.The carbomer is carbomer 910.The glycoprotein is Swine serum mucoprotein.It is described Phosphatide is soybean lecithin.
Example 4
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;After sepiolite ball milling, 500 mesh sieve is crossed, and is 1 in mass ratio by the sepiolite after sieving and organic acid soln:20 It is 55kHz in supersonic frequency after mixing, under the conditions of temperature is 55 DEG C, ultrasonic immersing 3h obtains maceration extract, and by gained maceration extract Rotary Evaporators are moved into, is 75 DEG C in temperature, under the conditions of pressure is 600kPa, 5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by institute No. 1 concentrate is obtained under the conditions of temperature is 95 DEG C, after dry 4h, is transferred to tube furnace, under the conditions of temperature is 400 DEG C, heat preservation roasts 60min is burnt, cools to room temperature with the furnace, discharges, obtains pretreatment sepiolite;Sepiolite then will be pre-processed and organic alkali solution presses matter Amount is than being 1:It is 55 DEG C in temperature after 15 mixing, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains reaction solution, and By gained reaction solution move into Rotary Evaporators, in temperature be 85 DEG C, pressure be 700kPa under the conditions of, be concentrated under reduced pressure 5h, obtain No. 2 it is dense Contracting liquid, and be 4h dry under the conditions of 90 DEG C in temperature by No. 2 concentrates of gained, obtain modified meerschaum;It counts in parts by weight, successively Take 10 parts of glycoprotein, 8 parts of phosphatide, 6 parts of carragheens, 300 parts of water first pour into phosphatide, carragheen and water in reaction kettle, in temperature It is 75 DEG C, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 4h, then glycoprotein is added in into reaction kettle, be with after temperature 85 DEG C, under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 5h, obtains mixed liquor;It is 1 in mass ratio:10 by modified meerschaum It is poured into batch mixer with mixed liquor, is 1200r/min in rotating speed, under the conditions of temperature is 75 DEG C, after constant temperature is stirred 6h, will mix Material is injected by syringe in mold in material machine, and mold is moved into refrigerator, and 8h is pre-chilled under the conditions of being -28 DEG C in temperature, The mold after precooling is moved into vacuum freezing drying oven again, is -48 DEG C in temperature, under the conditions of pressure is 30Pa, vacuum refrigeration is done Dry 36h, discharging, demoulds to get composite aerogel type cigarette filter tip materials.The organic alkali solution is that mass fraction is 15% Tetrapropylammonium hydroxide solution.The glycoprotein is Swine serum mucoprotein.The phosphatide is soybean lecithin.
Example 5
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;After sepiolite ball milling, 500 mesh sieve is crossed, and is 1 in mass ratio by the sepiolite after sieving and organic acid soln:20 It is 55kHz in supersonic frequency after mixing, under the conditions of temperature is 55 DEG C, ultrasonic immersing 3h obtains maceration extract, and by gained maceration extract Rotary Evaporators are moved into, is 75 DEG C in temperature, under the conditions of pressure is 600kPa, 5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by institute No. 1 concentrate is obtained under the conditions of temperature is 95 DEG C, after dry 4h, is transferred to tube furnace, under the conditions of temperature is 400 DEG C, heat preservation roasts 60min is burnt, cools to room temperature with the furnace, discharges, obtains pretreatment sepiolite;Sepiolite then will be pre-processed and organic alkali solution presses matter Amount is than being 1:It is 55 DEG C in temperature after 15 mixing, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains reaction solution, and By gained reaction solution move into Rotary Evaporators, in temperature be 85 DEG C, pressure be 700kPa under the conditions of, be concentrated under reduced pressure 5h, obtain No. 2 it is dense Contracting liquid, and be 4h dry under the conditions of 90 DEG C in temperature by No. 2 concentrates of gained, obtain modified meerschaum;It counts in parts by weight, successively Take 40 parts of carbomers, 10 parts of glycoprotein, 8 parts of phosphatide, 300 parts of water first pour into carbomer, phosphatide and water in reaction kettle, Yu Wen It is 75 DEG C to spend, and under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 4h, then glycoprotein is added in into reaction kettle, with after temperature It it is 85 DEG C, under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 5h, obtains mixed liquor;It is 1 in mass ratio:10 will modified Hai Pao Stone and mixed liquor are poured into batch mixer, are 1200r/min in rotating speed, under the conditions of temperature is 75 DEG C, after constant temperature is stirred 6h, are incited somebody to action Material is injected by syringe in mold in batch mixer, and mold is moved into refrigerator, is pre-chilled under the conditions of being -28 DEG C in temperature 8h, then by after precooling mold move into vacuum freezing drying oven, in temperature be -48 DEG C, pressure be 30Pa under the conditions of, vacuum refrigeration Dry 36h, discharging are demoulded to get composite aerogel type cigarette filter tip materials.The organic alkali solution is that mass fraction is 15% tetrapropylammonium hydroxide solution.The carbomer is carbomer 910.The glycoprotein is Swine serum mucoprotein.The phosphorus Fat is soybean lecithin.
Example 6
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;After sepiolite ball milling, 500 mesh sieve is crossed, and is 1 in mass ratio by the sepiolite after sieving and organic acid soln:20 It is 55kHz in supersonic frequency after mixing, under the conditions of temperature is 55 DEG C, ultrasonic immersing 3h obtains maceration extract, and by gained maceration extract Rotary Evaporators are moved into, is 75 DEG C in temperature, under the conditions of pressure is 600kPa, 5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by institute No. 1 concentrate is obtained under the conditions of temperature is 95 DEG C, after dry 4h, is transferred to tube furnace, under the conditions of temperature is 400 DEG C, heat preservation roasts 60min is burnt, cools to room temperature with the furnace, discharges, obtains pretreatment sepiolite;Sepiolite then will be pre-processed and organic alkali solution presses matter Amount is than being 1:It is 55 DEG C in temperature after 15 mixing, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains reaction solution, and By gained reaction solution move into Rotary Evaporators, in temperature be 85 DEG C, pressure be 700kPa under the conditions of, be concentrated under reduced pressure 5h, obtain No. 2 it is dense Contracting liquid, and be 4h dry under the conditions of 90 DEG C in temperature by No. 2 concentrates of gained, obtain modified meerschaum;It counts in parts by weight, successively Take 40 parts of carbomers, 8 parts of phosphatide, 6 parts of carragheens, carbomer, phosphatide, carragheen and water first pours into reaction kettle by 300 parts of water In, it is 75 DEG C in temperature, under the conditions of supersonic frequency is 55kHz, after ultrasonic disperse 4h, with being 85 DEG C after temperature, rotating speed is Under the conditions of 800r/min, constant temperature is stirred to react 5h, obtains mixed liquor;It is 1 in mass ratio:10 pour into modified meerschaum and mixed liquor In batch mixer, it is 1200r/min in rotating speed, under the conditions of temperature is 75 DEG C, after constant temperature is stirred 6h, material in batch mixer is led to It crosses in syringe injection mold, and mold is moved into refrigerator, 8h is pre-chilled, then will be after precooling under the conditions of being -28 DEG C in temperature Mold moves into vacuum freezing drying oven, is -48 DEG C in temperature, under the conditions of pressure is 30Pa, vacuum freeze drying 36h discharges, and takes off Mould is to get composite aerogel type cigarette filter tip materials.The organic alkali solution is the tetrapropyl hydroxide that mass fraction is 15% Ammonium salt solution.The carbomer is carbomer 910.The phosphatide is soybean lecithin.
Example 7
It is 3 in mass ratio:1:20 pour into oxalic acid, citric acid and water in beaker, with glass bar stirring and dissolving 30min, obtain organic Acid solution;After sepiolite ball milling, 500 mesh sieve is crossed, and is 1 in mass ratio by the sepiolite after sieving and organic acid soln:20 It is 55kHz in supersonic frequency after mixing, under the conditions of temperature is 55 DEG C, ultrasonic immersing 3h obtains maceration extract, and by gained maceration extract Rotary Evaporators are moved into, is 75 DEG C in temperature, under the conditions of pressure is 600kPa, 5h is concentrated under reduced pressure, obtains No. 1 concentrate, and by institute No. 1 concentrate is obtained under the conditions of temperature is 95 DEG C, after dry 4h, is transferred to tube furnace, under the conditions of temperature is 400 DEG C, heat preservation roasts 60min is burnt, cools to room temperature with the furnace, discharges, obtains pretreatment sepiolite;Sepiolite then will be pre-processed and organic alkali solution presses matter Amount is than being 1:It is 55 DEG C in temperature after 15 mixing, under the conditions of rotating speed is 600r/min, constant temperature is stirred to react 4h, obtains reaction solution, and By gained reaction solution move into Rotary Evaporators, in temperature be 85 DEG C, pressure be 700kPa under the conditions of, be concentrated under reduced pressure 5h, obtain No. 2 it is dense Contracting liquid, and be 4h dry under the conditions of 90 DEG C in temperature by No. 2 concentrates of gained, obtain modified meerschaum;It counts in parts by weight, successively Taking 40 parts of carbomers, 10 parts of glycoprotein, 6 parts of carragheens, 300 parts of water first pour into carbomer, carragheen and water in reaction kettle, In temperature be 75 DEG C, supersonic frequency be 55kHz under the conditions of, after ultrasonic disperse 4h, then glycoprotein is added in into reaction kettle, with after Temperature is 85 DEG C, and under the conditions of rotating speed is 800r/min, constant temperature is stirred to react 5h, obtains mixed liquor;It is 1 in mass ratio:10 will be modified Sepiolite and mixed liquor are poured into batch mixer, are 1200r/min in rotating speed, under the conditions of temperature is 75 DEG C, constant temperature is stirred 6h Afterwards, material in batch mixer is injected by syringe in mold, and mold is moved into refrigerator, under the conditions of temperature is -28 DEG C Be pre-chilled 8h, then by after precooling mold move into vacuum freezing drying oven, in temperature be -48 DEG C, pressure be 30Pa under the conditions of, vacuum 36h is freeze-dried, discharging is demoulded to get composite aerogel type cigarette filter tip materials.The organic alkali solution is mass fraction For 15% tetrapropylammonium hydroxide solution.The carbomer is carbomer 910.The glycoprotein is Swine serum mucoprotein.
Comparative example:Take certain commercially available brand cigarette.
The composite aerogel type cigarette filter tip materials of 1 to 7 gained of example and comparative example product are subjected to performance detection, tool Body detecting method is as follows:
1. absorption property:According to GB/T 19609 to the burst size of tar(Single branch)It is detected;According to GB/T 23228 to Asia Nitramine class flue gas(Single branch)Burst size be detected;
2. mechanical property:The hardness of test specimen is detected according to YC/T223.2.
Specific testing result is as shown in table 1:
Table 1
By 1 testing result of table it is found that the composite aerogel type cigarette filter tip materials of technical solution of the present invention preparation are with excellent Absorption property, to the adsorption effect outstanding feature of harmful substance in cigarette, and with preferable mechanical property, and can retain The fragrance of cigarette has broad prospects in the development of cigarette filter material industry.

Claims (7)

1. a kind of preparation method of composite aerogel type cigarette filter tip materials, it is characterised in that specifically preparation process is:
(1)It is 1 in mass ratio by sepiolite and organic acid soln:10~1:After 20 mixing, ultrasonic immersing, then through being concentrated under reduced pressure, Dry, roasting obtains pretreatment sepiolite;
(2)It is 1 in mass ratio that sepiolite, which will be pre-processed, with organic alkali solution:10~1:After 15 mixing, constant temperature is stirred to react, then is passed through It is concentrated under reduced pressure, it is dry, obtain modified meerschaum;
(3)It counts in parts by weight, takes 30~40 parts of carbomers, 8~10 parts of glycoprotein, 6~8 parts of phosphatide, 4~6 parts of OK a karaoke clubs successively Carbomer, phosphatide and carragheen, are first added to the water by glue, 200~300 parts of water, after ultrasonic disperse, add glycoprotein, constant temperature It is stirred to react, obtains mixed liquor;
(4)It is 1 in mass ratio:8~1:After 10 are stirred modified meerschaum and mixed liquor constant temperature, inject in mold, then pass through After low temperature precooling, vacuum freeze drying is demoulded to get composite aerogel type cigarette filter tip materials.
2. a kind of preparation method of composite aerogel type cigarette filter tip materials according to claim 1, it is characterised in that: Step(1)It is 3 in mass ratio by oxalic acid, citric acid and water that the organic acid soln, which is,:1:20 are configured.
3. a kind of preparation method of composite aerogel type cigarette filter tip materials according to claim 1, it is characterised in that: Step(2)The organic alkali solution is the tetrapropylammonium hydroxide solution that mass fraction is 10~15%.
4. a kind of preparation method of composite aerogel type cigarette filter tip materials according to claim 1, it is characterised in that: Step(3)The carbomer is carbomer 910, any one in carbomer 934 or Acritamer 940.
5. a kind of preparation method of composite aerogel type cigarette filter tip materials according to claim 1, it is characterised in that: Step(3)The glycoprotein is any one in Swine serum mucoprotein, cow's serum mucoprotein or chicken serum mucoprotein.
6. a kind of preparation method of composite aerogel type cigarette filter tip materials according to claim 1, it is characterised in that: Step(3)The phosphatide is any one in soybean lecithin or egg lecithin.
7. a kind of preparation method of composite aerogel type cigarette filter tip materials according to claim 1, it is characterised in that: Step(4)The low temperature is pre-chilled:Under the conditions of temperature is -30~-28 DEG C, 6~8h is pre-chilled.
CN201711278092.XA 2017-12-06 2017-12-06 A kind of preparation method of composite aerogel type cigarette filter tip materials Pending CN108158034A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109463796A (en) * 2018-10-10 2019-03-15 湖北中烟工业有限责任公司 A kind of glass fiber toughened composite aerogel and preparation method thereof
CN110200317A (en) * 2019-05-08 2019-09-06 中山市博海精细化工有限公司 A kind of low viscosity cigarette filter filler and preparation method

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Publication number Priority date Publication date Assignee Title
CN1376433A (en) * 2001-03-22 2002-10-30 周永璋 Molecular sieve for cigarette
CN101172243A (en) * 2006-11-01 2008-05-07 中国石油化工股份有限公司 Mesoporous material/micropore molecular sieve composite material and preparation method thereof
CN102423132A (en) * 2011-08-15 2012-04-25 武汉力诚生物科技有限公司 Plant polysaccharide cigarette filter tip and preparation method thereof
CA2871808A1 (en) * 2012-05-03 2013-11-07 British American Tobacco (Investments) Limited Improvements in smoking article filters
CN107199015A (en) * 2017-06-29 2017-09-26 滁州卷烟材料厂 A kind of preparation method of sepiolite base volume cigarette filter tip adsorbent

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1376433A (en) * 2001-03-22 2002-10-30 周永璋 Molecular sieve for cigarette
CN101172243A (en) * 2006-11-01 2008-05-07 中国石油化工股份有限公司 Mesoporous material/micropore molecular sieve composite material and preparation method thereof
CN102423132A (en) * 2011-08-15 2012-04-25 武汉力诚生物科技有限公司 Plant polysaccharide cigarette filter tip and preparation method thereof
CA2871808A1 (en) * 2012-05-03 2013-11-07 British American Tobacco (Investments) Limited Improvements in smoking article filters
CN107199015A (en) * 2017-06-29 2017-09-26 滁州卷烟材料厂 A kind of preparation method of sepiolite base volume cigarette filter tip adsorbent

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109463796A (en) * 2018-10-10 2019-03-15 湖北中烟工业有限责任公司 A kind of glass fiber toughened composite aerogel and preparation method thereof
CN110200317A (en) * 2019-05-08 2019-09-06 中山市博海精细化工有限公司 A kind of low viscosity cigarette filter filler and preparation method

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