Cellulose diacetate tube and melt extrusion formula, method and application thereof

Abstract

The invention discloses a cellulose diacetate tube and a melt extrusion formula, method and application thereof. The cellulose diacetate tube comprises cellulose diacetate, glycerol triacetate, polyethylene glycol, an antioxidant and a whitening agent. The cellulose diacetate tube is prepared from 50-80 parts by mass of cellulose diacetate, 10-30 parts by mass of glycerol triacetate, 5-30 parts by mass of polyethylene glycol, 0.1-2 parts by mass of an antioxidant and 0.1-5 parts by mass of a whitening agent. The cellulose diacetate tube prepared from the formula, the method and the application can meet the whiteness and hardness standards of filter tubes for cigarettes.

Description

Technical Field

[0001] This invention belongs to the field of polymer material processing technology, and relates to a cellulose diacetate tube and its melt extrusion formulation, method and application. Background Technology

[0002] Cellulose acetate was the first cellulose derivative to be commercially produced. Based on the degree of substitution, cellulose acetate can be classified into monoacetate, diacetate, and triacetate. Due to its strong thermal stability, diacetate is widely used in cigarette filters and textile fibers; over 85% of countries worldwide use it as a material for cigarette filters [Zhang Q, Fang C, Cheng Y, et al. Construction and properties of cellulose diacetate film derived from waste cigarette filters. Cellulose, 2020, 27: 8899-8907; Shan Weiwei, Zhou Zhihong. Production, application and market of cellulose acetate. Acetaldehyde Acetic Acid Chemicals, 2016, 4: 15-21.]. Currently, cellulose diacetate is generally processed using solution spinning, which requires dissolving cellulose diacetate in acetone to form a slurry, followed by complex processes such as spinning, crimping, and drying [Li Pengxiang, Wu Shaohua, Yang Zhanping, et al. Research progress on spinning process and properties of cellulose diacetate tow. Industrial Textiles, 2014, 32(2):8-12; Tang Aimin, Chen Gang, Wu Shubin, et al. Study on rheological properties of cellulose diacetate acetone solution. Cellulose Science and Technology, 2001, 9(3): 11-18.]. This production process is an intensive process integrating chemical, textile, and thermoelectric industries, involving many harmful media and a long process, and is highly dangerous.

[0003] Melt processing of polymer materials involves heating the material above its melting point, transforming it from a solid to a viscous flow state. The fluidity of this viscous flow polymer is then utilized to achieve the molding and processing of the material. Melt processing does not involve the use of solvents, effectively solving the problems currently faced in solution spinning of cellulose diacetate. However, cellulose diacetate molecules contain numerous hydroxyl and acetyl groups, which can form hydrogen bonds between the chains, resulting in strong intermolecular forces. During melt processing, cellulose diacetate is difficult to flow and prone to degradation, thus affecting the application of cellulose diacetate materials and making it difficult to meet the whiteness and hardness standards for cigarette filter tubes. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide a cellulose diacetate tube and its melt extrusion formulation, method and application. The cellulose diacetate tube obtained by the formulation, method and application can meet the whiteness and hardness standards of tobacco filter tubes.

[0005] To achieve the above objectives, the present invention discloses a melt extrusion formulation for cellulose diacetate tubes, comprising cellulose diacetate, triacetyl ester, polyethylene glycol, antioxidant, and whitening agent.

[0006] Furthermore, the mass fractions of cellulose diacetate, triacetyl ester, polyethylene glycol, antioxidant, and whitening agent are 50-80 parts, 10-30 parts, 5-30 parts, 0.1-2 parts, and 0.1-5 parts, respectively.

[0007] Furthermore, the plasticizer is triacetin or polyethylene glycol.

[0008] Furthermore, the whitening agent is either German Ventor or Japanese Fuji Titanium TA301.

[0009] Furthermore, the antioxidant is antioxidant 1076, antioxidant 1010, or antioxidant 1098.

[0010] This invention discloses a melt extrusion method for cellulose diacetate tubes, comprising the following steps: 1) Mix cellulose diacetate, triacetyl ester, polyethylene glycol, antioxidant and whitening agent evenly to obtain a mixture; 2) The mixture is added to an extruder and extruded through a tubular extrusion die at a preset extrusion temperature and screw speed to obtain cellulose diacetate tubes.

[0011] Furthermore, in step 2), the temperatures of temperature control zone 1, temperature control zone 2, temperature control zone 3 and temperature control zone 4 of the extruder are 60 ºC ~ 140 ºC, 140 ºC ~ 200 ºC, 150 ºC ~ 200 ºC, and 130 ºC ~ 180 ºC, respectively.

[0012] Furthermore, in step 2), the preset screw speed is 50 r / min ~ 600 r / min; In step 2), the outer diameter of the tubular extrusion die device is 5~10 mm and the inner diameter is 3~8 mm.

[0013] This invention discloses a cellulose diacetate tube, which is prepared by melt extrusion method based on the cellulose diacetate tube.

[0014] This invention discloses the application of cellulose diacetate tube in the preparation of cigarette filters.

[0015] The present invention has the following beneficial effects: In the specific operation of the cellulose diacetate tube, its melt extrusion formulation, method, and application described in this invention, a plasticizer is used to physically modify the cellulose diacetate, lowering its glass transition temperature. Simultaneously, an antioxidant is used to increase the decomposition temperature of the cellulose diacetate, broadening its melt processing temperature range. A whitening agent is used to increase the whiteness of the cellulose diacetate extrudate. Through a reasonable extrusion formulation and process design, and with the aid of a tubular die device, the melt extrusion of the cellulose diacetate tube is achieved, meeting the whiteness and hardness standards for cigarette filter tubes. Testing shows that the cellulose diacetate tube prepared by this invention has a whiteness higher than 80, an adjustable hardness over a wide range (Shore hardness 30~70HA), excellent mechanical properties, and a ring stiffness of 25~200 kN / m. 2 It is adjustable and can be compressed to 10% without causing damage. Attached Figure Description

[0016] To more clearly illustrate the technical solutions of the embodiments of this application, the drawings used in the description of the embodiments of this application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 Differential scanning calorimetry (DSC) curves of cellulose diacetate plasticized with triacetyl ester and polyethylene glycol as shown in Examples 1, 2, 3 and 4, and cellulose diacetate plasticized with no plasticizer and single plasticizer as shown in Comparative Examples 1, 2, 3 and Belgium. Figure 2 The diagram shows the compressive stress-strain curves and ring stiffness values ​​of the triacetyl glycerol and polyethylene glycol composite plasticized cellulose diacetate tubes shown in Examples 1, 3 and 4. Figure 3 The whiteness and Shore hardness distribution of cellulose acetate tubes shown in Examples 1, 2, 3, 4, 5, 6, 7, 8, 9, Comparative Examples 2, 3, 4, 5, 6, 7, 8, 9 and 10 are shown in the diagram. Detailed Implementation The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0018] In the description of this invention, it should be understood that the terms "comprising" and "including" indicate the presence of the described features, integrals, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or collections thereof.

[0019] It should also be understood that the terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. As used in this specification and the appended claims, the singular forms “a,” “an,” and “the” are intended to include the plural forms unless the context clearly indicates otherwise.

[0020] It should also be further understood that the term "and / or" as used in this specification and the appended claims refers to any combination and all possible combinations of one or more of the associated listed items, and includes such combinations. For example, A and / or B can represent three cases: A alone, A and B simultaneously, and B alone. Additionally, the character " / " in this invention generally indicates that the preceding and following objects have an "or" relationship.

[0021] It should be understood that although terms such as first, second, third, etc., may be used in the embodiments of the present invention to describe the preset range, these preset ranges should not be limited to these terms. These terms are only used to distinguish the preset ranges from one another. For example, without departing from the scope of the embodiments of the present invention, the first preset range may also be referred to as the second preset range, and similarly, the second preset range may also be referred to as the first preset range.

[0022] Depending on the context, the word "if" as used here can be interpreted as "when," "when," "in response to determination," or "in response to detection." Similarly, depending on the context, the phrase "if determination" or "if detection (of the stated condition or event)" can be interpreted as "when determination," "in response to determination," "when detection (of the stated condition or event)," or "in response to detection (of the stated condition or event)."

[0023] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0024] The accompanying drawings illustrate various structural schematic diagrams according to embodiments disclosed in this invention. These drawings are not to scale, and some details have been enlarged for clarity, and some details may have been omitted. The shapes of the various regions and layers shown in the drawings, as well as their relative sizes and positional relationships, are merely exemplary and may deviate from reality due to manufacturing tolerances or technical limitations. Furthermore, those skilled in the art can design regions / layers with different shapes, sizes, and relative positions as needed.

[0025] The melt extrusion method for cellulose diacetate tubes of the present invention includes the following steps: Mix 50-80 parts of cellulose diacetate, 10-30 parts of triacetyl ester, 5-30 parts of polyethylene glycol, 0.1-2 parts of antioxidant, and 0.1-5 parts of whitening agent until homogeneous. Dry under vacuum at a constant temperature. Finally, extrude the cellulose diacetate tube through an extruder at a preset screw speed and a tubular die. The specific steps include: 1) Mix 50-80 parts of cellulose diacetate, 10-30 parts of triacetyl ester, 5-30 parts of polyethylene glycol, 0.1-2 parts of antioxidant and 0.1-5 parts of whitening agent until homogeneous to obtain a mixture; 2) The mixture is added to an extruder and extruded through a tubular extrusion die at a preset extrusion temperature and screw speed to obtain cellulose diacetate tubes.

[0026] In this embodiment, in step 2), the temperatures of temperature control zone 1, temperature control zone 2, temperature control zone 3, and temperature control zone 4 of the extruder are 60 ºC ~ 140 ºC, 140 ºC ~ 200 ºC, 150 ºC ~ 200 ºC, and 130 ºC ~ 180 ºC, respectively.

[0027] In this embodiment, in step 2), the preset screw speed is 50 r / min ~ 600 r / min.

[0028] In this embodiment, in step 2), the outer diameter of the tubular extrusion die device is 5~10 mm and the inner diameter is 3~8 mm.

[0029] In this embodiment, the plasticizer is triacetin or polyethylene glycol.

[0030] In this embodiment, the whitening agent is either German VENTOR or Japanese Fuji Titanium TA301. The German VENTOR has an average particle size of 0.4 micrometers, a coating layer, a whiteness of 98.1, and a pH value of 8.1. The Japanese Fuji Titanium TA301 has an average particle size of 0.6 micrometers, a whiteness of 97.7, and a pH value of 7.0.

[0031] In this embodiment, the antioxidant is antioxidant 1076, antioxidant 1010, or antioxidant 1098.

[0032] It should be noted that during melt extrusion, the addition of plasticizers significantly reduces the melt viscosity of cellulose diacetate, allowing it to be extruded at lower processing temperatures and imparting excellent flexibility to cellulose diacetate. The addition of antioxidants effectively prevents thermal degradation of cellulose diacetate during extrusion. The addition of whitening agents imparts excellent whiteness to the cellulose diacetate tubes. Cellulose diacetate tubes prepared using the extrusion formulation and process have a smooth surface, uniform wall thickness, high whiteness (>80), and adjustable hardness (Shore hardness 30~70 HA).

[0033] The cellulose diacetate tube obtained by this invention can be used in the field of cigarette filters. The cellulose diacetate tube is filled with cellulose diacetate filaments, and its mechanical properties and draw resistance are tested.

[0034] Example 1 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 74:10:10:1:5; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 140 ºC, 200 ºC, 200 ºC and 180 ºC respectively. The screw speed is 50 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 5 mm and an inner diameter of 3 mm.

[0035] Example 2 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 70:20:5:2:3; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 120 ºC, 175 ºC, 190 ºC, and 170 ºC respectively. The screw speed is 100 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0036] Example 3 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076, and whitening agent VENTOR evenly in a mass ratio of 67.9:25:5:0.1:2; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 100 ºC, 170 ºC, 185 ºC, and 170 ºC respectively. The screw speed is 150 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0037] Example 4 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076, and whitening agent VENTOR evenly in a mass ratio of 55.5:35:5:0.5:4; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 80 ºC, 170 ºC, 180 ºC, and 170 ºC respectively. The screw speed is 200 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0038] Example 5 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 70:10:15:1:4; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 100 ºC, 190 ºC, 190 ºC, and 180 ºC respectively. The screw speed is 100 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 10 mm and an inner diameter of 7 mm.

[0039] Example 6 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 55:25:15:2:3; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 85 ºC, 165 ºC, 175 ºC, and 165 ºC respectively. The screw speed is 300 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0040] Example 7 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1010 and whitening agent TA301 evenly in a mass ratio of 55:25:16:1:3; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 70 ºC, 160 ºC, 175 ºC, and 165 ºC respectively. The screw speed is 200 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0041] Example 8 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1098 and whitening agent TA301 evenly in a mass ratio of 55:20:20:1:4; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 95 ºC, 165 ºC, 180 ºC, and 160 ºC respectively. The screw speed is 300 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0042] Example 9 The specific operation of this embodiment is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1076, and whitening agent TA301 evenly in a mass ratio of 50:17.5:30:0.5:2; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 90 ºC, 160 ºC, 170 ºC, and 160 ºC respectively. The screw speed is 500 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0043] Comparative Example 1 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 98:1:1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 120 ºC, 220 ºC, 210 ºC, and 190 ºC respectively, and the screw speed is 200 r / min. The cellulose diacetate extrusion formulation cannot be extruded from the tubular extrusion die device.

[0044] Comparative Example 2 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, polyethylene glycol, antioxidant 1098 and whitening agent TA301 evenly in a mass ratio of 88:10:1:0.1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 150 ºC, 225 ºC, 215 ºC, and 200 ºC respectively. The screw speed is 100 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0045] Comparative Example 3 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 88:10:1:1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 150 ºC, 220 ºC, 215 ºC, and 200 ºC, respectively. The screw speed is 50 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0046] Comparative Example 4 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, antioxidant 1098 and whitening agent TA301 evenly in a mass ratio of 83:15:1:1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 150 ºC, 220 ºC, 215 ºC, and 195 ºC, respectively. The screw speed is 75 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0047] Comparative Example 5 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, triacetyl glycerol, antioxidant 1076 and whitening agent TA301 evenly in a mass ratio of 78:20:1:1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 160 ºC, 205 ºC, 205 ºC and 190 ºC respectively, and the screw speed is 200 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0048] Comparative Example 6 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, polyethylene glycol, antioxidant 1076, and whitening agent TA301 evenly in a ratio of 79:20:0.5:0.5; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 155 ºC, 205 ºC, 200 ºC, and 185 ºC respectively. The screw speed is 300 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0049] Comparative Example 7 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, polyethylene glycol, antioxidant 1076 and whitening agent VENTOR evenly in a mass ratio of 79:20:0.5:0.5; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 150 ºC, 190 ºC, 200 ºC, and 180 ºC respectively. The screw speed is 200 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0050] Comparative Example 8 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, polyethylene glycol, antioxidant 1076 and whitening agent TA301 evenly in a mass ratio of 69:30:0.5:0.1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 130 ºC, 175 ºC, 185 ºC, and 170 ºC respectively. The screw speed is 100 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0051] Comparative Example 9 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1010 and whitening agent VENTOR evenly in a mass ratio of 69:9:21:0.5:0.5; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 140 ºC, 180 ºC, 190 ºC, and 170 ºC respectively. The screw speed is 250 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0052] Comparative Example 10 The specific operation for this comparative example is as follows: S1, mix cellulose diacetate raw material, triacetyl ester, polyethylene glycol, antioxidant 1096 and whitening agent TA301 evenly in a mass ratio of 73:5:20:1:1; S2, the cellulose diacetate extrusion formulation is added to the extruder, and the temperatures of the extruder temperature control zones one to four are controlled at 150 ºC, 180 ºC, 190 ºC, and 175 ºC respectively. The screw speed is 300 r / min. The cellulose diacetate tube is obtained by melt extrusion through the tubular extrusion die device of the extruder with an outer diameter of 7 mm and an inner diameter of 5 mm.

[0053] To investigate the plasticizing effect of this invention on cellulose diacetate, differential scanning calorimetry was first performed on Examples 1, 2, 3, and 4, as well as Comparative Examples 1, 2, 3, and 4. The test results are as follows: Figure 1 As shown, from Figure 1As can be seen, in Comparative Example 1, without plasticizer, cellulose diacetate could not be melt-extruded, and the glass transition temperature was 181 °C. The glass transition temperatures of the cellulose diacetate extrusion formulations in Comparative Examples 2, 3, and 4 were 175 °C, 170 °C, and 162 °C, respectively. The single plasticizer extrusion formulation could reduce the glass transition temperature of cellulose diacetate to some extent, achieving melt extrusion, but the melt extrusion effect was poor, and the extrudate showed significant degradation. In contrast, the extrusion formulations in Examples 1, 2, 3, and 4, under the synergistic plasticizing effect of the composite plasticizer, significantly reduced the glass transition temperature of cellulose diacetate to 156 °C, 149 °C, 130 °C, and 108 °C, respectively. The extrusion effect of cellulose diacetate was good, the surface quality of the extrudate was good, and there was no obvious degradation. This indicates that the cellulose diacetate melt extrusion formulation of the present invention exhibits excellent processability, can significantly reduce the glass transition temperature of cellulose diacetate, and increase the fluidity of the cellulose diacetate melt extrusion process. Meanwhile, the extrusion formulation also increases the degradation temperature of cellulose diacetate, broadens the processing temperature range of cellulose diacetate, effectively avoids thermal degradation during the melt extrusion process of cellulose diacetate, and ensures the excellent surface quality and mechanical properties of the cellulose diacetate extrudate.

[0054] To investigate the mechanical properties of the cellulose diacetate tubular materials, compression mechanical properties were tested using a compressive strength tester for Examples 1, 3, and 4. The test results are as follows: Figure 2 As shown, Figure 2 As shown in Figure a, by designing different plasticizer formulations, it is possible to prepare both softer tubes with lower elastic modulus, as in Example 4, and harder tubes with higher elastic modulus, as in Example 1. In summary, through the extrusion formulation design described in this invention, cellulose diacetate tubes with a wide range of adjustable mechanical properties can be prepared. Further calculations were performed on the ring stiffness of the cellulose diacetate tubes. S for:

[0055] in, F The force value is relative to the tube's 3.0% compression deformation, and the unit is kilonewton (kN). L The length of the pipe is in meters (m). Y The deformation of the tube when compressed by 3.0% is expressed in meters (m). Y / d = 0.03, d For example, the inner diameter of the pipe. Figure 2 As shown in b, the ring stiffness of Examples 1, 3, and 4 is between 25 and 177 kN / m. 2 It is adjustable over a wide range.

[0056] To examine the surface quality and hardness of the cellulose diacetate tube of the present invention, whiteness and Shore hardness tests were performed on the products obtained in Examples 1, 2, 3, 4, 5, 6, 7, 8, 9, Comparative Examples 2, 3, 4, 5, 6, 7, 8, 9, and 10. The test results are as follows: Figure 3 As shown, by Figure 3 It can be seen that the cellulose diacetate tube melt extrusion formulation and process described in this invention can prepare cellulose diacetate tubes with high whiteness (>80) and a wide range of adjustable Shore hardness (30~70 HA); while the cellulose diacetate tubes prepared by Comparative Examples 2, 3, 4, 5, 6, 7, 8, 9 and 10 all have low whiteness (<32), and the melt extrusion process causes more serious degradation.

[0057] In summary, the cellulose diacetate tube for tobacco produced by this invention has a good melt extrusion effect, solves the problem of melt processing of cellulose diacetate, and produces a cellulose diacetate tube with high whiteness and adjustable mechanical properties over a wide range.

[0058] Other embodiments of the invention will readily occur to those skilled in the art upon consideration of the specification and disclosure of the invention. This application is intended to cover any variations, uses, or adaptations of the invention that follow the general principles of the invention and include common knowledge or customary techniques in the art not disclosed herein. The specification and examples are to be considered exemplary only, and the true scope and spirit of the invention are indicated by the following claims.

[0059] It should be understood that the present invention is not limited to the precise structure described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of the invention is limited only by the appended claims.

[0060] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation on the present invention. Any simple modifications, alterations, or equivalent structural changes made to the above embodiments based on the technical essence of the present invention shall still fall within the protection scope of the present invention.

Claims

1. A melt-extrusion formulation of a cellulose diacetate tube, characterized in that, Cellulose diacetate, triacetin, polyethylene glycol, antioxidant and whitening agent.

2. The melt-extruded formulation of a cellulose diacetate tube according to claim 1, characterized in that, The mass fractions of cellulose diacetate, triacetin, polyethylene glycol, antioxidant and whitening agent are 50-80 parts, 10-30 parts, 5-30 parts, 0.1-2 parts and 0.1-5 parts respectively.

3. The melt-extruded formulation of cellulose bisulphate tubing according to claim 1, characterised in that, The plasticizer is triacetin or polyethylene glycol.

4. The melt-extruded formulation of cellulose bisulphate tubing according to claim 1, characterised in that, The whitening agent is German Pantone VENTOR or Japanese Fuji Titanium TA301.

5. The melt-extruded formulation of cellulose diacetate tubing according to claim 1, wherein, The antioxidant is antioxidant 1076, antioxidant 1010 or antioxidant 1098.

6. A melt-extrusion method of a cellulose diacetate tube, characterized by, The method comprises the following steps: 1) uniformly mix cellulose diacetate, triacetin, polyethylene glycol, antioxidant and whitening agent to obtain a mixture; 2) add the mixture into an extruder, extrude through a tubular extrusion die device at a preset extrusion temperature and screw rotation speed to obtain a cellulose diacetate tube.

7. The method of claims 6, wherein the cellulosic diacetate tubing is extruded at a temperature of from about 150°C to about 200°C. In step 2), the temperatures of the temperature control zone 1, the temperature control zone 2, the temperature control zone 3 and the temperature control zone 4 of the extruder are 60-140 °C, 140-200 °C, 150-200 °C and 130-180 °C respectively.

8. The method of claim 6, wherein the cellulosic diacetate tubing is formed by melt extrusion. In step 2), the preset screw rotation speed is 10-600 r / min. In step 2), the outer diameter of the tubular extrusion die device is 5-10 mm and the inner diameter is 3-8 mm.

9. A cellulose diacetate tube characterized by, Prepared based on the method of any one of claims 6-8.

10. Use of the cellulose diacetate tube of claim 9 in the field of preparing cigarette filters.

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