WO2022099902A1

WO2022099902A1 - Method for measuring lip sticking force of tipping paper for cigarettes according to magnitude of contact angle

Info

Publication number: WO2022099902A1
Application number: PCT/CN2020/141623
Authority: WO
Inventors: 杨继; 刘志华; 向能军; 刘春波; 朱瑞芝; 司晓喜; 唐石云; 何沛; 张凤梅; 蒋薇; 杨晨; 蒋昆明; 李振杰
Original assignee: 云南中烟工业有限责任公司
Priority date: 2020-11-10
Filing date: 2020-12-30
Publication date: 2022-05-19
Also published as: CN112198094A

Abstract

A method for measuring the lip sticking force of tipping paper for cigarettes. The degree of a contact angle θ formed by droplets of artificial saliva on a surface of the tipping paper for cigarettes is measured by using a contact angle meter, and then, a quantitative relationship between the magnitude of the contact angle θ and the lip sticking force of the tipping paper for cigarettes is established, such that the magnitude of the lip sticking force of the tipping paper for cigarettes can be determined. According to the method, the quantitative relationship of the consistency between the measurement result of the degree of the contact angle θ formed by droplets of artificial saliva on the surface of the tipping paper for cigarettes and the lip sticking force of the tipping paper for cigarettes is established for the first time, and the extent of lip sticking of the tipping paper is quantified. Compared with a manual suction evaluation result, the method has greatly enhanced reproducibility.

Description

A kind of method for measuring lip sticking force of cigarette tipping paper according to the size of contact angle

technical field

The invention belongs to the technical field of tobacco testing, and in particular relates to a method for measuring the lip sticking force of cigarette tipping paper according to the size of the contact angle.

Background technique

The cigarette filter is mainly composed of three layers of acetate fiber, forming paper and tipping paper. The tipping paper, also known as tipping paper, is used to wrap around the filter tip and bond the filter tip to the end of the tobacco rod. The tipping paper is a kind of decorative paper obtained by printing, coating and other processing on the base paper. It is usually cork color or opaque white, and has the effect of improving the appearance. The tipping paper is in direct contact with the smoker's lips. When the weather is dry, when consumers smoke cigarettes, there may be a small amount of saliva that will moisten the tipping paper, and then slowly dry during smoking, leaving saliva proteins on the lips. It will have a bonding effect on the tipping paper, which will cause the tipping paper on the filter tip to stick to the skin of the lips, and even stick to the lips, causing tearing and bleeding. After smoking, the filter tip cannot be spit out smoothly, which seriously affects the cigarette consumption experience. feel. A good tipping paper should not stick to the lips during suction.

At present, the research hotspots of cigarette filter tipping paper at home and abroad mostly focus on its pyrolysis properties, low ignition properties, harmful element content, modification of cigarette paper and the release ability of modified carbon monoxide, toxicity and safety evaluation etc. However, there is no relevant research on the screening or judgment of its sticky lip strength. The lip sticking aspect is all about improving the formulation and process of the butt-loading paper, and there is no specific screening method or judgment method. For example, the invention patent "a fragrance and health tipping paper that prevents the lips and tongue from drying out and its preparation method" describes the technological formula of tipping paper, but only the longitudinal tensile strength and air permeability of the base paper are detected in the effect test. , there is no mention of whether there is a sticky lip force. The utility model patent "a filter with anti-sticking lip and anti-pollution" is coated with a protective film on the tipping paper and "a multifunctional tipping paper" for the purpose of anti-sticking lip, fragrance, flame retardant, etc. The outer layer of the pine paper is compounded with a fruit fragrance waterproof layer and a protective film layer, but the judgment result of the anti-stick lip is not mentioned. There is no corresponding standard in the industry to regulate, and major enterprises rely only on professional evaluation and judgment, which has great subjectivity and uncertainty. In order to determine whether different processes and different types of tipping paper are sticky to the lips It is urgent to establish corresponding objective screening and detection methods.

The lip-sticking degree of the tipping paper, the evaluation method of the prior art is: in the manual suction process, the lip-sticking degree is qualitatively scored by the subjective feeling of the sucker, and then whether the lip-sticking performance of the tipping paper is given. qualified. The disadvantage of this evaluation method is that it is completely based on artificial subjective feeling, and the reproducibility is poor; and the results cannot be strictly quantified.

The present invention uses the contact angle measurement method for the evaluation of the lip-sticking force of the tipping paper for the first time, and establishes a quantitative relationship of the consistency between the measurement result of the contact angle and the lip-sticking force of the cigarette tipping paper, so that the lip-sticking force of the tipping paper is The degree of stickiness was quantified. Compared with manual aspiration, the reproducibility is greatly enhanced.

SUMMARY OF THE INVENTION

The purpose of the present invention is to establish a method for measuring the lip sticking force of cigarette tipping paper. The method of the invention uses a contact angle tester to test the contact angle formed by the droplets of artificial saliva on the surface of the cigarette tipping paper, and then establishes a quantitative relationship between the contact angle and the lip sticking force of the cigarette tipping paper.

The technical scheme of the present invention is as follows:

The invention discloses a method for measuring the lip sticking force of cigarette tipping paper. A contact angle tester is used to test the degree of contact angle θ formed by the droplets of artificial saliva on the surface of cigarette tipping paper, as shown in FIG. 2 , Then, the quantitative relationship between the angle of the contact angle θ and the lip-sticking force of the cigarette tipping paper can be established, and the lip-sticking force of the cigarette tipping paper can be judged.

Preferably, the contact angle tester includes the following components:

-- rack plane 1;

--The storage workbench 2 is located in the middle of the frame plane 1, and the storage workbench 2 is controlled by the workbench forward and backward movement knob 3 and the workbench up and down movement knob 4;

--Backlight screen 6, located in the vertical direction of the side surface of the storage workbench 2, the brightness of the backlight screen 6 is controlled by the brightness adjustment knob 5;

-- The camera 12 is located on the other side of the storage table 2, the camera 12, the storage table 2 and the backlight screen 6 are roughly on a horizontal line, and the camera 12 faces the storage table 2 and the backlight screen 6; The height of the camera 12 is slightly higher than the table top of the storage workbench 2;

--Sampling rack 13, located on the upper part of the storage workbench 2, on which there is a sampling syringe 11, the sampling syringe 11 is vertically arranged so that the needle head of the sampling syringe 11 is facing the The table top of the storage workbench 2; the sample injection needle cylinder 11 has a sample injection liquid injection knob 10 at the bottom; Angle fine-tuning knob 9 control.

Preferably, the testing steps for testing the angle of the contact angle formed by the droplets of artificial saliva on the surface of the tipping paper for cigarettes are as follows:

① Arrange artificial saliva, and then put it into the sampling syringe 11; place the sample of cigarette tipping paper on the table top of the storage workbench 2; adjust the height and the left and right positions of the storage workbench 2 to make the cigarette use The tipping paper sample is located at the center of the image of the camera 12; the height of the sampling syringe 11 is adjusted so that the needle is about 2.0 mm away from the surface of the cigarette tipping paper sample;

②A drop of artificial saliva with a volume of 2 μL is dropped from the sample injection syringe 11. When the artificial saliva is in complete contact with the surface of the cigarette tipping paper sample, the injection needle is separated from the drop, and the timing is started, and the contact time does not exceed 4 minute;

3. The contact angle θ of the artificial saliva droplets on the surface of the cigarette tipping paper sample is measured and calculated respectively, and each cigarette tipping paper sample is measured 5 times;

④ Make statistics on the test data of step ③, the test result is expressed as the average value of 5 measurements, and the angle degree of the contact angle θ is accurate to 0.1°.

Preferably, the lip-adhesion force of the cigarette tipping paper is manually evaluated, and then a quantitative relationship between the magnitude of the contact angle and the lip-adhesion force of the cigarette tipping paper is established.

Preferably, the composition of the artificial saliva is as shown in the following table:

reagent	Concentration (g/l)
Magnesium chloride (MgCl ₂ .6H ₂ O)	0.17
Calcium chloride (GaCl ₂ .2H ₂ O)	0.15
Potassium dihydrogen phosphate (K ₂ HPO ₄ 2H ₂ O)	0.76
Potassium carbonate (K ₂ CO ₃ )	0.53
Sodium Chloride (NaCl)	0.33
Potassium Chloride (KCl)	0.75
Hydrochloric acid (HCl, mass fraction is 1%)	Add to pH 6.8±0.1

.

Preferably, the method for measuring the contact angle of the sample of cigarette tipping paper is the hanging drop method, and the steps are as follows: measuring the diameter 2r of the spherical crown of the droplet formed on the surface of the sample of cigarette tipping paper and the diameter of the spherical crown by measuring the artificial saliva. For the height h, the contact angle in degrees is calculated according to the following formula: θ=2tan ^-1 (h/r).

Determination method Hanging drop method, also called θ/2 method, as shown in Figure 3, artificial saliva forms droplets on the surface of the cigarette tipping paper sample, due to the surface tension of the liquid itself and the cigarette tipping paper. Due to the effect of surface free energy, the liquid will tend to form a spherical cap. The diameter 2r of the test liquid and the height h of the spherical cap can be obtained by analyzing the width of the left and right points and the height of the arc in the side elevational view of the image. The value of the contact angle θ can be calculated by θ=2tan ⁻¹ (h/r); since point m and point p are the tangent points, θ ₁ =θ ₂ =θ ₃ , θ=θ ₁ +θ ₃ .

Preferably, the definition: when the degree of contact angle θ formed by the droplets of artificial saliva on the surface of the cigarette tipping paper is ≥ 100°, the lip stickiness grade of the cigarette tipping paper is determined to be grade 0, which means that it does not stick to the lips. ; When 90°≤θ<100°, determine the lip stickiness of cigarette tipping paper as grade 1, showing mild lip stickiness; when 80°≤θ<90°, determine the lip stickiness of cigarette tipping paper The grade result is grade 2, showing moderate lip stickiness; when 70°≤θ<80°, the lip stickiness grade of cigarette tipping paper is determined to be grade 3, showing severe lip stickiness; when θ<70°, it is determined The lip stickiness grade of cigarette tipping paper was grade 4, which showed severe stickiness.

Beneficial effects of the present invention:

1. The present invention uses the contact angle measurement method for the evaluation of the lip-sticking force of tipping paper for the first time, and establishes the measurement result of the contact angle θ formed by the droplets of artificial saliva on the surface of the cigarette tipping paper. The quantitative relationship of the consistency between the lip-sticking force of the tipping paper quantifies the lip-sticking degree of the tipping paper. The reproducibility is greatly enhanced compared to the results compared with manual aspiration.

2. The composition of the artificial saliva of the present invention is close to the composition of the saliva secreted by the human body, and the consistency of the quantitative relationship between the degree of the contact angle θ measured using the artificial saliva of the present invention and the sticking force of the cigarette tipping paper is good .

3. The first definition of the present invention: when the degree of contact angle θ formed by the droplets of artificial saliva on the surface of the cigarette tipping paper is ≥ 100°, the result of the lip stickiness of the cigarette tipping paper is determined to be grade 0, which means that it is not. Sticky lips; when 90°≤θ<100°, determine the lip stickiness grade of cigarette tipping paper to be grade 1, showing mild lip stickiness; when 80°≤θ<90°, determine that the cigarette tipping paper is sticky. The lip grade result is grade 2, which is moderately sticky lips; when 70°≤θ<80°, the lip stickiness grade result of cigarette tipping paper is determined to be grade 3, which shows severe lip stickiness; when θ<70° , to determine the lip stickiness grade of cigarette tipping paper is 4, showing severe stickiness. This definition provides those skilled in the art with the idea of quantifying the lip-sticking force of cigarette tipping paper.

Description of drawings

FIG. 1 is a schematic diagram of the contact angle tester of the present invention.

The reference signs are: 1. Rack; 2. Object storage workbench; 3. Back and forth movement knob of the storage workbench; 4. Up and down movement knob of the object storage workbench; 5. Backlight screen brightness adjustment knob; Left and right adjustment knobs of sample rack; 8. Left and right adjustment knobs of sampling rack; 9. Fine adjustment knob of sampling rack angle; 10. Knob of injection liquid injection; 11. Sampling syringe; 12. Industrial camera;

2 is a schematic diagram of the contact angle θ formed by the droplets of the artificial saliva of the present invention on the surface of the tipping paper for cigarettes. The left picture shows that the contact angle θ is less than 90°, and the right picture shows that the contact angle θ is greater than 90°.

The reference signs are: Y, the spherical cap of the artificial saliva; Z, the tipping paper for cigarettes.

3 is a schematic diagram of the calculation of the contact angle θ formed by the droplets of the artificial saliva of the present invention on the surface of the tipping paper for cigarettes.

Detailed ways

In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described below with reference to specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention. The experimental methods that do not specify specific conditions in the following examples are generally in accordance with conventional conditions. Unless otherwise specified, the percentages and parts are by weight.

The invention discloses a method for measuring the lip sticking force of cigarette tipping paper. A contact angle tester is used to test the contact angle θ formed by droplets of artificial saliva on the surface of cigarette tipping paper, as shown in FIG. 2 . , and then establish the quantitative relationship between the angle of the contact angle θ and the lip sticking force of the cigarette tipping paper, and then the lip sticking force of the cigarette tipping paper can be judged. The contact angle tester, as shown in Figure 1, includes the following components: a frame plane 1; The working table is moved up and down by the knob 4; the backlight screen 6 is located in the vertical direction of the side of the storage workbench 2, and the brightness of the backlight screen 6 is controlled by the brightness adjustment knob 5; the camera 12 is located in the storage workbench 2. On the other side, the camera 12, the storage table 2 and the backlight screen 6 are roughly on a horizontal line, and the camera 12 faces the storage table 2 and the backlight screen 6; the height of the camera 12 is slightly higher than the height of the storage table 2. table top; the sample injection rack 13 is located on the upper part of the storage workbench 2, and there is a sample injection syringe 11 on it. The table top of the storage workbench 2; the sample injection needle cylinder 11 has a sample injection liquid injection knob 10 at the bottom; Angle fine-tuning knob 9 control.

Using the contact angle tester as shown in FIG. 1 to test the angle of the contact angle formed by the droplets of artificial saliva on the surface of the tipping paper for cigarettes, the test steps are as follows:

Then the lip-sticking force of the cigarette tipping paper was manually evaluated, and then the quantitative relationship between the contact angle and the lip-sticking force of the cigarette tipping paper was established.

The composition of the artificial saliva is shown in the following table:

试剂reagent	浓度(g/l)Concentration (g/l)
氯化镁(MgCl ₂.6H ₂O) Magnesium chloride (MgCl ₂ .6H ₂ O)	0.170.17
氯化钙(GaCl ₂.2H ₂O) Calcium chloride (GaCl ₂ .2H ₂ O)	0.150.15
磷酸二氢钾(K ₂HPO _4·2H ₂O) Potassium dihydrogen phosphate (K ₂ HPO ₄ 2H ₂ O)	0.760.76
碳酸钾(K ₂CO ₃) Potassium carbonate (K ₂ CO ₃ )	0.530.53
氯化钠(NaCl)Sodium Chloride (NaCl)	0.330.33
氯化钾(KCl)Potassium Chloride (KCl)	0.750.75
盐酸(HCl,质量分数为1％)Hydrochloric acid (HCl, mass fraction is 1%)	添加至PH为6.8±0.1Add to pH 6.8±0.1

The method for measuring the contact angle of the cigarette tipping paper sample is the pendant drop method. The contact angle in degrees is calculated as follows: θ = 2tan ^-1 (h/r). Determination method Hanging drop method, also called θ/2 method, as shown in Figure 3, artificial saliva forms droplets on the surface of the cigarette tipping paper sample, due to the surface tension of the liquid itself and the cigarette tipping paper. Due to the effect of surface free energy, the liquid will tend to form a spherical cap. The diameter 2r of the test liquid and the height h of the spherical cap can be obtained by analyzing the width of the left and right points and the height of the arc in the side elevational view of the image. The value of the contact angle θ can be calculated by θ=2tan ⁻¹ (h/r); since points m and p are tangent points, θ ₁ =θ ₂ =θ ₃ , θ=θ ₁ +θ ₃ .

According to the test results, the definition is: when the contact angle θ formed by the droplets of artificial saliva on the surface of the cigarette tipping paper is greater than or equal to 100°, the lip stickiness grade of the cigarette tipping paper is determined to be grade 0, indicating that it is not sticky. lip; when 90°≤θ<100°, determine the lip stickiness grade of cigarette tipping paper to be grade 1, showing mild lip stickiness; when 80°≤θ<90°, determine that cigarette tipping paper sticks to the lip The result of the sex grade is grade 2, showing moderate lip stickiness; when 70°≤θ<80°, the lip stickiness grade result of cigarette tipping paper is determined to be grade 3, showing severe lip stickiness; when θ<70°, The lip stickiness grade of cigarette tipping paper was determined to be grade 4, showing severe stickiness.

Example 1

In this embodiment, 20 different samples are detected by the method of the present invention and the existing manual suction evaluation method, and the detection results are shown in the following table. Among them, the manual evaluation adopts multiple groups of coded dark evaluation, that is, if the evaluation personnel do not know the contact angle of the sample in advance, the same sample is divided into multiple groups of random codes, and the evaluation personnel can evaluate the suction and give a grade: non-sticky lips, light There are five grades of lip stickiness, moderate lip stickiness, severe lip stickiness, and severe lip stickiness; among them, lip stickiness is grade 1 for mild lip stickiness, grade 2 for moderate lip stickiness, and grade 3 for severe lip stickiness and lip stickiness. Grade 4 is severe sticky lips.

Example 2

In this embodiment, 20 different samples are also detected by the method of the present invention and the existing manual suction evaluation method, and the detection results are shown in the following table. Among them, manual evaluation of suction also uses multiple groups of coded dark evaluations.

From the test results of Example 1 and Example 2, it can be known that the detection method of the present invention is completely consistent with the manual evaluation of suction detection results. The method of the invention can objectively and accurately quantify whether the cigarette tipping paper has the lip sticking force, is easy to popularize and apply, and provides a basis for the standard formulation of the cigarette sticking force.

The foregoing has shown and described the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above-mentioned embodiments, and the descriptions in the above-mentioned embodiments and the description are only to illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have Various changes and modifications fall within the scope of the claimed invention. The claimed scope of the present invention is defined by the appended claims and their equivalents.

Claims

A method for measuring the lip sticking force of cigarette tipping paper, characterized in that, a contact angle tester is used to test the degree of the contact angle θ formed by the droplets of artificial saliva on the surface of the cigarette tipping paper, and then the contact angle θ is established. The quantitative relationship between the size of the angle and the lip-sticking force of the cigarette tipping paper can determine the lip-sticking force of the cigarette tipping paper.
The method for measuring the lip sticking force of cigarette tipping paper according to claim 1, wherein the contact angle tester comprises the following components:

--Rack plane(1);

--The storage workbench (2) is located in the middle of the frame plane (1), and the storage workbench (2) is controlled by the workbench forward and backward movement knob (3) and the workbench up and down movement knob (4);

--backlight screen (6), located in the vertical direction of the side surface of the storage workbench (2), the brightness of the backlight screen (6) is controlled by the brightness adjustment knob (5);

-- a camera (12), located on the other side of the storage table (2), the camera (12), the storage table (2) and the backlight screen (6) are roughly on a horizontal line, and the camera (12) ) facing the storage table (2) and the backlight screen (6); the height of the camera (12) is slightly higher than the table top of the storage table (2);

--Sampling rack (13), located on the upper part of the storage workbench (2), on which there is a sampling syringe (11), the sampling syringe (11) is arranged vertically so that the sampling needle The needle head of the barrel (11) faces the table top of the storage workbench (2); the sample injection needle barrel (11) has a sample injection liquid injection knob (10) at the bottom; the sample injection rack (13) is provided by the inlet The sample rack left and right adjustment knob (7), the sample rack left and right adjustment knob (8) and the sample rack angle fine adjustment knob (9) control.
The method for measuring the lip sticking force of cigarette tipping paper according to claim 2, wherein the test steps of the angle of the contact angle formed by the droplet of the test artificial saliva on the surface of the cigarette tipping paper are as follows:

① Prepare artificial saliva, and then put it into the sampling syringe (11); place the sample of cigarette tipping paper on the table top of the storage workbench (2); adjust the height and the height of the storage workbench (2). position the cigarette tipping paper sample at the center of the image of the camera (12); adjust the height of the sampling syringe (11) so that the needle is about 2.0mm away from the surface of the cigarette tipping paper sample ;

② A drop of artificial saliva with a volume of 2 μL is dropped from the sample injection syringe (11). When the artificial saliva is in complete contact with the surface of the cigarette tipping paper sample, the injection needle is separated from the drop, and the timing is started. more than 4 minutes;

3. The contact angle θ of the artificial saliva droplets on the surface of the cigarette tipping paper sample is measured and calculated respectively, and each cigarette tipping paper sample is measured 5 times;

④ Make statistics on the test data of step ③, the test result is expressed as the average value of 5 measurements, and the angle degree of the contact angle θ is accurate to 0.1°.
The method for measuring the lip-sticking force of cigarette tipping paper according to claim 3, wherein the lip-sticking force of cigarette tipping paper is manually evaluated, and then the size of the contact angle and the lip-sticking force of cigarette tipping paper are established. Quantitative relationship between sticky lip forces.
The assay method of cigarette tipping paper sticking force according to claim 3, is characterized in that, the composition of described artificial saliva is as shown in the following table:

reagent Concentration (g/l) Magnesium chloride (MgCl 2 .6H 2 O) 0.17 Calcium chloride (GaCl 2 .2H 2 O) 0.15 Potassium dihydrogen phosphate (K 2 HPO 4 2H 2 O) 0.76 Potassium carbonate (K 2 CO 3 ) 0.53 Sodium Chloride (NaCl) 0.33 Potassium Chloride (KCl) 0.75 Hydrochloric acid (HCl, mass fraction is 1%) Add to pH 6.8±0.1

.
The method for measuring the lip sticking force of cigarette tipping paper according to claim 3, wherein the method for measuring the contact angle of the cigarette tipping paper sample is the high method of hanging drop, and the steps are as follows: measure the artificial saliva in the The diameter 2r of the spherical cap of the droplet and the height h of the spherical cap are formed on the surface of the cigarette tipping paper sample, and the contact angle is calculated according to the following formula: θ=tan −1 (h/r).
The method for measuring lip sticking force of cigarette tipping paper according to claim 1, characterized in that: when the degree of contact angle θ formed by the droplets of artificial saliva on the surface of cigarette tipping paper is ≥100°, The lip stickiness grade of cigarette tipping paper is determined to be grade 0, which means that it does not stick to the lip; when 90°≤θ<100°, the lip stickiness grade of cigarette tipping paper is determined to be grade 1, which shows slight stickiness. When 80°≤θ<90°, the lip stickiness grade of cigarette tipping paper is determined to be grade 2, showing moderate lip stickiness; when 70°≤θ<80°, it is determined that cigarette tipping paper sticks to the lip. The result of the sex grade is 3, showing severe lip sticking; when θ<70°, the lip stickiness grade of cigarette tipping paper is determined to be 4, showing severe lip sticking.