CN110903619A - Preparation method of modified PLA cooling material - Google Patents
Preparation method of modified PLA cooling material Download PDFInfo
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- CN110903619A CN110903619A CN201911100801.4A CN201911100801A CN110903619A CN 110903619 A CN110903619 A CN 110903619A CN 201911100801 A CN201911100801 A CN 201911100801A CN 110903619 A CN110903619 A CN 110903619A
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- Prior art keywords
- modified pla
- preparation
- placing
- solid
- modified
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- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000001816 cooling Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 241000208125 Nicotiana Species 0.000 claims abstract description 15
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 15
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 40
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 239000007787 solid Substances 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 12
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 10
- 229960001701 chloroform Drugs 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229920006381 polylactic acid film Polymers 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000779 smoke Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 235000019505 tobacco product Nutrition 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 235000019504 cigarettes Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/664—Polyesters containing oxygen in the form of ether groups derived from hydroxy carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
Abstract
The invention relates to the technical field of manufacturing of tobacco materials, and provides a preparation method of a modified PLA cooling material.
Description
Technical Field
The invention relates to the technical field of manufacturing of tobacco materials, in particular to a preparation method of a modified PLA cooling material, and the modified PLA cooling material can be applied to a novel tobacco filter rod section.
Background
With the rapid development of new tobacco products, various big tobacco companies have introduced related products in the market. However, the length of the novel tobacco filter rod segment is shorter than that of a conventional cigarette, and the position of the heating source is closer to the filter rod segment, so that various novel tobacco products on the market exist at present, and the smoke temperature at the tail end of the filter rod is overhigh in the using process. The traditional filament bundle used as the filter stick material can not meet the requirement of novel tobacco cooling, and how to reduce the smoke temperature of the filter stick section of the novel tobacco product becomes a problem which is urgently needed to be solved by various big tobacco companies and cigarette bullet manufacturers.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a modified PLA cooling material, and the modified PLA cooling material can be applied to a novel tobacco filter rod section, plays a role in cooling smoke and has certain mechanical properties. The invention uses PLA material as raw material, which is modified by adding montmorillonite, polyethylene glycol, etc., to improve the heat resistance and mechanical property of the material, and prepares modified PLA film by film forming, which not only facilitates adding in the section of novel tobacco filter stick, but also ensures normal resistance of novel tobacco product.
The technical scheme adopted by the invention is as follows:
a preparation method of a modified PLA cooling material comprises the following steps:
(1) weighing 30-50mL of 70wt% toluene, placing the toluene into a test tube, adding 5-17g of polyethylene glycol, placing the test tube into an oil bath for heat preservation, controlling the temperature at 105-120 ℃, boiling and refluxing for 6h, then carrying out reduced pressure evaporation, removing the toluene and water in the test tube, and obtaining dry polyethylene glycol for later use;
(2) taking a 500mL beaker as a reaction vessel, adding 45-70mL of dimethylbenzene, adding 3-13g of lactide and 6-9g of PLA, uniformly stirring, then adding 5-10mL of 12mg/L stannous octoate, heating at 40-65 ℃, simultaneously gradually adding the dehydrated polyethylene glycol obtained in the step (1), slowly raising the temperature of the oil bath to 120 ℃ and 145 ℃, continuously stirring, after the reaction is finished, distilling the dimethylbenzene under reduced pressure, mixing the obtained product with trichloromethane according to the mass ratio of 1:4.5, precipitating by using methanol, and filtering to obtain a white modified PLA solid;
(3) weighing 5g of modified PLA solid, placing the modified PLA solid into a conical flask, adding 20ml of 6mg/L trichloromethane, adding 0.3-0.8g of montmorillonite after the modified PLA solid is dissolved, shaking the conical flask to mix the powder, then placing the conical flask into an ultrasonic instrument for ultrasonic treatment for 1h, placing the obtained suspension on a polytetrafluoroethylene plate, and volatilizing the liquid at room temperature to obtain the modified PLA film added with the montmorillonite.
Further, the obtained modified PLA solid is physically blended with other high molecular substances to prepare a film, and the film is added into the tobacco filter stick.
Further, the other high molecular substance is polyethylene, polypropylene, or the like.
Further, the obtained modified PLA solid is mixed with glass fiber or resin material by using a mould pressing process to prepare the cylindrical composite material.
The modified PLA cooling material prepared by the method can be applied to a novel tobacco filter rod segment, plays a role in cooling smoke and has certain mechanical properties. The invention uses PLA material as raw material, which is modified by adding montmorillonite, polyethylene glycol, etc., to improve the heat resistance and mechanical property of the material, and prepares modified PLA film by film forming, which not only facilitates adding in the section of novel tobacco filter stick, but also ensures normal resistance of novel tobacco product.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention.
Example 1
A preparation method of a modified PLA cooling material comprises the following steps:
(1) preparation of dried polyethylene glycol: 40ml of toluene (70 wt%) is weighed, 6g of polyethylene glycol is added, the mixture is uniformly mixed, and then the mixture is placed into an oil bath pan at 110 ℃ for heat preservation for 6 hours and is dried under reduced pressure.
(2) Putting 60ml of dimethylbenzene (anhydrous grade, standard solution, purity 99%), 8g of lactide and 8g of PLA into a beaker for blending, adding 7ml of stannous octoate (12 mg/L) serving as a catalyst after uniformly stirring, keeping the temperature of an oil bath at 50 ℃, slowly adding the dried polyethylene glycol obtained in the step (1), raising the temperature of the oil bath to 125 ℃ after adding, continuing stirring, carrying out reduced pressure distillation after reaction is finished, mixing the obtained product with trichloromethane according to the mass ratio of 1:4.5, and precipitating by using methanol to obtain a primary modified PLA solid.
(3) Dissolving 5g of modified PLA solid into 20ml of trichloromethane (6 mg/L), adding 0.6g of montmorillonite, uniformly mixing, carrying out ultrasonic treatment for 1h, placing the obtained suspension on a polytetrafluoroethylene plate, and drying to form a film, thus obtaining the modified PLA film added with the montmorillonite.
Example 2
A preparation method of a modified PLA cooling material comprises the following steps:
(1) preparation of dried polyethylene glycol: 30ml of toluene (70 wt%) is weighed, 5g of polyethylene glycol is added, after uniform mixing, the mixture is placed in an oil bath pan at 105 ℃ for heat preservation for 6h, and reduced pressure drying is carried out.
(2) Putting 45ml of dimethylbenzene (anhydrous grade, standard solution, purity 99%), 3g of lactide and 6g of PLA into a beaker for blending, uniformly stirring, adding 5ml of stannous octoate (12 mg/L) serving as a catalyst, keeping the temperature of an oil bath at 50 ℃, slowly adding the dried polyethylene glycol obtained in the step (1), raising the temperature of the oil bath to 120 ℃ after the addition is finished, continuing stirring, carrying out reduced pressure distillation after the reaction is finished, mixing the obtained product with trichloromethane according to the mass ratio of 1:4.5, and precipitating by using methanol to obtain a primary modified PLA solid.
(3) Dissolving 5g of modified PLA solid into 20ml of trichloromethane (6 mg/L), adding 0.6g of montmorillonite, uniformly mixing, carrying out ultrasonic treatment for 1h, placing the obtained suspension on a polytetrafluoroethylene plate, and drying to form a film, thus obtaining the modified PLA film added with the montmorillonite.
Example 3
A preparation method of a modified PLA cooling material comprises the following steps:
(1) preparation of dried polyethylene glycol: 50ml of toluene (70 wt%) is weighed, 17g of polyethylene glycol is added, after uniform mixing, the mixture is placed in an oil bath kettle at 120 ℃ for heat preservation for 6h, and reduced pressure drying is carried out.
(2) Putting 70ml of dimethylbenzene (anhydrous grade, standard solution, purity 99%), 13g of lactide and 9g of PLA into a beaker for blending, adding 10ml of stannous octoate (12 mg/L) serving as a catalyst after uniformly stirring, keeping the temperature of an oil bath at 65 ℃, slowly adding the dried polyethylene glycol obtained in the step (1), raising the temperature of the oil bath to 145 ℃ after the addition is finished, continuing stirring, carrying out reduced pressure distillation after the reaction is finished, mixing the obtained product with trichloromethane according to the mass ratio of 1:4.5, and precipitating by using methanol to obtain a primary modified PLA solid.
(3) Dissolving 5g of modified PLA solid into 20ml of trichloromethane (6 mg/L), adding 0.6g of montmorillonite, uniformly mixing, carrying out ultrasonic treatment for 1h, placing the obtained suspension on a polytetrafluoroethylene plate, and drying to form a film, thus obtaining the modified PLA film added with the montmorillonite.
Test of cooling effect
The modified PLA film prepared in example 1 was laminated and added to a novel tobacco filter rod, and the smoke end temperature of the filter rod was measured by a thermocouple, with the results shown in table 1.
TABLE 1 indexes and end flue gas temperatures of modified PLA film filter sticks and pure tow filter sticks
The experimental results show that the novel tobacco filter stick made of the modified PLA cooling material meets all basic indexes of filter stick making, and has obvious cooling effect on the tail end smoke temperature.
Details not described in this specification are within the skill of the art that are well known to those skilled in the art.
The invention is not to be considered as limited to the particular embodiments shown and described, but is to be understood that all changes, equivalents, and modifications that come within the spirit and scope of the invention are desired to be protected.
Claims (4)
1. A preparation method of a modified PLA cooling material is characterized by comprising the following steps:
(1) weighing 30-50mL of 70wt% toluene, placing the toluene into a test tube, adding 5-17g of polyethylene glycol, placing the test tube into an oil bath for heat preservation, controlling the temperature at 105-120 ℃, boiling and refluxing for 6h, then carrying out reduced pressure evaporation, removing the toluene and water in the test tube, and obtaining dry polyethylene glycol for later use;
(2) taking a 500mL beaker as a reaction vessel, adding 45-70mL of dimethylbenzene, adding 3-13g of lactide and 6-9g of PLA, uniformly stirring, then adding 5-10mL of 12mg/L stannous octoate, heating at 40-65 ℃, simultaneously gradually adding the dehydrated polyethylene glycol obtained in the step (1), slowly raising the temperature of the oil bath to 120 ℃ and 145 ℃, continuously stirring, after the reaction is finished, distilling the dimethylbenzene under reduced pressure, mixing the obtained product with trichloromethane according to the mass ratio of 1:4.5, precipitating by using methanol, and filtering to obtain a white modified PLA solid;
(3) weighing 5g of modified PLA solid, placing the modified PLA solid into a conical flask, adding 20ml of 6mg/L trichloromethane, adding 0.3-0.8g of montmorillonite after the modified PLA solid is dissolved, shaking the conical flask to mix the powder, then placing the conical flask into an ultrasonic instrument for ultrasonic treatment for 1h, placing the obtained suspension on a polytetrafluoroethylene plate, and volatilizing the liquid at room temperature to obtain the modified PLA film added with the montmorillonite.
2. The preparation method of the modified PLA cooling material according to claim 1, which is characterized in that: and physically blending the obtained modified PLA solid with other high molecular substances to prepare a film, and adding the film into the tobacco filter stick.
3. The preparation method of the modified PLA cooling material according to claim 2, which is characterized in that: the other high molecular substance is polyethylene or polypropylene.
4. The preparation method of the modified PLA cooling material according to claim 1, which is characterized in that: the obtained modified PLA solid is mixed with glass fiber or resin material by using a mould pressing process to prepare the cylindrical composite material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911100801.4A CN110903619B (en) | 2019-11-12 | 2019-11-12 | Preparation method of modified PLA cooling material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911100801.4A CN110903619B (en) | 2019-11-12 | 2019-11-12 | Preparation method of modified PLA cooling material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110903619A true CN110903619A (en) | 2020-03-24 |
| CN110903619B CN110903619B (en) | 2022-03-08 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911100801.4A Active CN110903619B (en) | 2019-11-12 | 2019-11-12 | Preparation method of modified PLA cooling material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110903619B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852124A (en) * | 2021-02-07 | 2021-05-28 | 云南长宜科技有限公司 | Cooling piece |
| CN114468354A (en) * | 2021-12-14 | 2022-05-13 | 江苏大亚滤嘴材料有限公司 | Preparation method of dust-free paper with cooling function and application of dust-free paper to composite filter stick |
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| CN108095195A (en) * | 2017-12-22 | 2018-06-01 | 安徽中烟工业有限责任公司 | A kind of aerosol generates article |
| CN108143004A (en) * | 2017-12-22 | 2018-06-12 | 安徽中烟工业有限责任公司 | It is a kind of to heat do not burn cigarette smoke cooling material and its application |
| CN108835710A (en) * | 2018-07-06 | 2018-11-20 | 武汉水木弘新材料有限公司 | A kind of flue-gas temperature is controllable, the incombustible cigarette filter rod of low temperature and preparation method thereof |
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-
2019
- 2019-11-12 CN CN201911100801.4A patent/CN110903619B/en active Active
Patent Citations (4)
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| CN108095195A (en) * | 2017-12-22 | 2018-06-01 | 安徽中烟工业有限责任公司 | A kind of aerosol generates article |
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Cited By (2)
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| CN112852124A (en) * | 2021-02-07 | 2021-05-28 | 云南长宜科技有限公司 | Cooling piece |
| CN114468354A (en) * | 2021-12-14 | 2022-05-13 | 江苏大亚滤嘴材料有限公司 | Preparation method of dust-free paper with cooling function and application of dust-free paper to composite filter stick |
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| Publication number | Publication date |
|---|---|
| CN110903619B (en) | 2022-03-08 |
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