A kind of preparation method of gingerol cellulose fiber

Abstract

The present invention belongs to the field of textile technology, and provides a method for preparing gingerol cellulose fiber, comprising at least the following steps: a preparation of gingerol oil-montmorillonite inclusion compound: gingerol oil is dissolved in ethanol for dispersion, then added dropwise to a sodium-montmorillonite suspension, and stirred at 78-82°C to form a gingerol oil-montmorillonite inclusion compound; b preparation of gingerol cellulose fiber: gingerol oil-montmorillonite inclusion compound is mixed with a cellulose viscose solution, and gingerol cellulose fiber is prepared by a wet spinning process. The present invention utilizes a sodium-montmorillonite sheet sandwich structure, and the dispersed gingerol oil is intercalated between the sodium-montmorillonite layers to form an inclusion compound, and the hydrophilicity of the sodium-montmorillonite is utilized to achieve uniform blending of the inclusion compound and the viscose solution, and gingerol cellulose fiber is prepared, and the gingerol coated with the sodium-montmorillonite is continuously preserved in the cellulose fiber, and the health care function of gingerol can be fully exerted.

Description

Technical Field

[0001] The invention relates to the technical field of textiles, and in particular to a method for preparing gingerol cellulose fiber. Background Art

[0002] With the advancement of science and technology, the improvement of people's consumption level and the enhancement of health awareness, functional fibers extracted from natural Chinese herbal medicine extracts and cellulose have realized the transformation from taking medicine to wearing clothes for protection and health prevention, and catered to people's various needs. Ginger is a tuberous rhizome of the ginger plant. As a traditional medicine and food plant, it contains three major components: volatile oil and gingerol diphenylheptane. Its sensory characteristics are mainly attributed to its two components: the aroma and part of the flavor of ginger depend on its volatile oil - essential oil, and the characteristic spicy flavor of ginger mainly comes from the non-volatile oil - gingerol in ginger oleoresin. The composition of gingerol is complex, mainly 4-gingerol, 6-gingerol, 8-gingerol, 10-gingerol, 12-gingerol, 6-shogaol, etc. The molecular structure of each component contains 3-methoxy-4-hydroxyphenyl functional group, which has strong antioxidant and natural antibacterial properties, has an excitatory effect on the vascular motor center, promotes blood circulation, and has medical and health care effects.

[0003] Patent CN201910720453.4 discloses a ginger health cellulose fiber and a preparation method thereof, wherein gingerol viscose fiber is spun by emulsifying and dispersing gingerol and adding it to a viscose solution, and gingerol is added to an oil bath before drying to increase the gingerol content of the fiber. This process causes a large amount of gingerol to be lost during the spinning process, and the gingerol added in the oiling process adheres to the fiber surface, has poor durability, and the fiber is light yellow. In addition, given that gingerol oil is difficult to be uniformly blended with a viscose aqueous solution of cellulose, and there is no chemical reaction between gingerol oil and cellulose, it is impossible to achieve the stable existence of gingerol in a cellulose matrix. Summary of the invention

[0004] Based on the above background technology, the present invention provides a method for preparing gingerol cellulose fiber, which utilizes the sandwich structure of sodium montmorillonite sheets to intercalate the dispersed gingerol oil into the sodium montmorillonite layers to form an inclusion compound, and utilizes the hydrophilicity of the sodium montmorillonite to achieve uniform blending of the inclusion compound and the viscose solution to prepare the gingerol cellulose fiber, and the gingerol coated with the sodium montmorillonite is continuously preserved in the cellulose fiber.

[0005] The present invention adopts the following technical solutions:

[0006] A method for preparing gingerol cellulose fiber comprises at least the following steps:

[0007] a Preparation of gingerol oil-montmorillonite inclusion complex: gingerol oil is dissolved in ethanol for dispersion, then added dropwise to the sodium montmorillonite suspension, and stirred at 78-82°C to react to form gingerol oil-montmorillonite inclusion complex;

[0008] b. Preparation of gingerol cellulose fiber: gingerol oil-montmorillonite inclusion complex is mixed with cellulose viscose solution, and gingerol cellulose fiber is prepared through wet spinning process.

[0009] Furthermore, in the above method for preparing gingerol cellulose fiber, the mass ratio of gingerol oil to ethanol in step a is 1:1-1:4.

[0010] Furthermore, in the above-mentioned method for preparing gingerol cellulose fiber, the sodium montmorillonite in step a is washed, and the washing process includes taking the sodium montmorillonite and deionized water at a ratio of 1:20-30, stirring and mixing, washing, and filtering several times, each stirring and washing time is 15-45 minutes, and the washing temperature is 78-82°C.

[0011] Furthermore, in the above method for preparing gingerol cellulose fiber, the concentration of the sodium montmorillonite suspension in step a is 5-10%.

[0012] Furthermore, in the above method for preparing gingerol cellulose fiber, the mass ratio of gingerol oil to sodium montmorillonite in step a is 1:5-10.

[0013] Furthermore, in the above method for preparing gingerol cellulose fiber, the gingerol oil-montmorillonite inclusion complex is further ground and dispersed after the reaction is completed in step a, and the particle size D90 of the system is ≤2 μm.

[0014] Furthermore, in the above method for preparing gingerol cellulose fiber, in step b, the mass ratio of sodium montmorillonite to cellulose is 1:20-30.

[0015] Furthermore, the method for preparing the gingerol cellulose fiber comprises the following steps:

[0016] a Preparation of gingerol oil-montmorillonite inclusion complex:

[0017] 1) Mix gingerol oil and ethanol in a mass ratio of 1:1-1:4;

[0018] 2) Mix sodium montmorillonite and deionized water at a ratio of 1:20-30, wash and filter for 3 times, each time for 30 minutes, and the washing temperature is controlled at 78-82°C;

[0019] 3) adding deionized water to the washed sodium montmorillonite to prepare a 5-10% suspension;

[0020] 4) Slowly drop gingerol oil dissolved in ethanol into the stirred and dispersed sodium montmorillonite suspension, the amount of drop is controlled according to the mass ratio of gingerol oil: sodium montmorillonite = 1:5-10, the temperature is controlled at 78-82°C, and the stirring is continued for 1-3h and then cooled to room temperature;

[0021] 5) adding the gingerol oil-montmorillonite inclusion complex suspension into a nano sand mill for grinding and dispersion, and stopping grinding when the system particle size D90 is ≤2 μm, and packaging for standby use to obtain the gingerol oil-montmorillonite inclusion complex;

[0022] b Preparation of gingerol cellulose fiber:

[0023] 1) Preparation of gingerol oil-montmorillonite inclusion complex and viscose blend solution

[0024] The same as the conventional viscose fiber production process, the cellulose viscose solution is prepared through pulp impregnation, pressing, crushing, aging, yellowing, dissolving, filtering, and degassing steps, the ground gingerol oil-montmorillonite inclusion compound is added to the viscose solution, homogenized and mixed evenly, and the amount of inclusion compound added is controlled by the mass ratio of sodium montmorillonite: cellulose = 1:20-30;

[0025] 2) Spinning and post-treatment of gingerol cellulose fibers

[0026] The gingerol oil-montmorillonite inclusion compound and viscose mixed solution are used to obtain fiber bundles through a wet spinning process, and the fiber bundles are stretched, cut, desulfurized, washed, oiled and dried to obtain gingerol cellulose fibers.

[0027] Furthermore, gingerol cellulose fiber is prepared by the above preparation method.

[0028] Furthermore, the mass percentage of gingerol in the gingerol cellulose fiber is ≥ 0.35%, and the content is detected by an extraction detection method.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] The invention provides a preparation method of gingerol cellulose fiber. The invention utilizes a montmorillonite layer sandwich structure, inserts dispersed gingerol oil into sodium-based montmorillonite layers to form an inclusion compound, utilizes the hydrophilicity of the montmorillonite to achieve uniform blending of the inclusion compound with a viscose solution to prepare the gingerol cellulose fiber. The gingerol coated with the sodium-based montmorillonite is continuously preserved in the cellulose fiber, thereby overcoming the difficulty that the traditional gingerol oil is difficult to be uniformly blended with a viscose solution of cellulose, and that the gingerol oil and cellulose do not chemically react, and that the gingerol cannot be stably present in a cellulose matrix. The mass percentage of gingerol in the prepared gingerol cellulose fiber is greater than or equal to 0.35%, and the health-care function of the gingerol can be fully exerted. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 Comparison of infrared spectra of gingerol cellulose fiber and regenerated cellulose fiber prepared in Example 1;

[0032] Figure 2 It is a comparison chart of the theoretical value and actual content of gingerol in Examples 1-4 and Comparative Examples. DETAILED DESCRIPTION

[0033] A method for preparing gingerol cellulose fiber comprises the following steps:

[0034] a Preparation of gingerol oil-montmorillonite inclusion complex:

[0035] 1) Mix gingerol oil and ethanol in a mass ratio of 1:1-1:4;

[0036] 2) Mix sodium montmorillonite and deionized water at a ratio of 1:20-30, wash and filter for 3 times, each time for 30 minutes, and the washing temperature is controlled at 78-82°C;

[0037] 3) adding deionized water to the washed sodium montmorillonite to prepare a 5-10% suspension;

[0038] 4) Slowly drop gingerol oil dissolved in ethanol into the stirred and dispersed sodium montmorillonite suspension, the amount of drop is controlled according to the mass ratio of gingerol oil: sodium montmorillonite = 1:5-10, the temperature is controlled at 78-82°C, and the stirring is continued for 1-3h and then cooled to room temperature;

[0039] 5) adding the gingerol oil-montmorillonite inclusion complex suspension into a nano sand mill for grinding and dispersion, and stopping grinding when the system particle size D90 is ≤2 μm, and packaging for standby use to obtain the gingerol oil-montmorillonite inclusion complex;

[0040] b Preparation of gingerol cellulose fiber:

[0041] 1) Preparation of gingerol oil-montmorillonite inclusion complex and viscose blend solution

[0042] The same as the conventional viscose fiber production process, the cellulose viscose solution is prepared through pulp impregnation, pressing, crushing, aging, yellowing, dissolving, filtering, and degassing steps, the ground gingerol oil-montmorillonite inclusion compound is added to the viscose solution, homogenized and mixed evenly, and the amount of inclusion compound added is controlled by the mass ratio of sodium montmorillonite: cellulose = 1:20-30;

[0043] 2) Spinning and post-treatment of gingerol cellulose fibers

[0044] The gingerol oil-montmorillonite inclusion compound and viscose mixed solution are used to obtain fiber bundles through a wet spinning process, and the fiber bundles are stretched, cut, desulfurized, washed, oiled and dried to obtain gingerol cellulose fibers.

[0045] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0046] Example 1

[0047] 1. Preparation of gingerol oil-montmorillonite inclusion complex

[0048] 1) Take 20g gingerol oil into a beaker, add 40g ethanol into the beaker, and stir to dissolve thoroughly.

[0049] 2) The washed sodium-montmorillonite is prepared into a 10% suspension, 1000 g of the suspension is weighed and added to a three-necked flask, and stirred, and the fully dissolved gingerol ethanol solution is dripped into the three-necked flask.

[0050] 3) The flask was heated with a heating jacket to 80°C, and the temperature was controlled at 80±2°C. Stirring was continued for 2 hours and then cooled to room temperature to obtain a suspension of gingerol oil: sodium montmorillonite inclusion complex in a ratio of 1:5.

[0051] 4) The gingerol oil-montmorillonite inclusion complex suspension was added into a nano sand mill for grinding and dispersion to obtain a suspension with a system particle size of D90 = 1.62 μm.

[0052] 2. Preparation of gingerol cellulose fiber

[0053] Take the viscose solution obtained by the production process of conventional viscose fiber, the viscose solution indicators are: cellulose content 8.8%, NaOH content 4.8%, viscosity 46s, maturity 16ml (10% NH4CL solution). Take 950g of the ground and dispersed gingerol oil-montmorillonite inclusion suspension and 20Kg of viscose solution, and blend them evenly with a homogenizer. The mixed viscose solution is used to obtain fiber bundles through a wet spinning process. The fiber bundles are drawn, cut, desulfurized, washed, oiled, and dried to obtain gingerol cellulose fibers. Refining is not bleached, and other process controls are the same as conventional viscose fibers.

[0054] The infrared spectra of the gingerol cellulose fiber prepared in this example and the regenerated cellulose fiber (without gingerol) were compared. Figure 1It can be seen that in addition to the characteristic infrared absorption peak of cellulose, the gingerol cellulose fiber also has a characteristic peak of gingerol (3-methoxy-4-hydroxyphenyl functional group) near 1452 cm-1, further indicating the presence of gingerol components in the fiber.

[0055] Example 2

[0056] 1. Preparation of gingerol oil-montmorillonite inclusion complex

[0057] 1) Take 10g gingerol oil into a beaker, add 20g ethanol into the beaker, and stir to dissolve thoroughly.

[0058] 2) The washed sodium-montmorillonite is prepared into a 10% suspension, 1000 g of the suspension is weighed and added to a three-necked flask, and stirred, and the fully dissolved gingerol ethanol solution is dripped into the three-necked flask.

[0059] 3) The flask was heated with a heating jacket to 80°C, and the temperature was controlled at 80±2°C. Stirring was continued for 2 hours and then cooled to room temperature to obtain a suspension of gingerol oil: sodium montmorillonite inclusion complex at a ratio of 1:10.

[0060] 4) The gingerol oil-montmorillonite inclusion complex suspension was added into a nano sand mill for grinding and dispersion to obtain a suspension with a system particle size of D90 = 1.37 μm.

[0061] 2. Preparation of gingerol cellulose fiber

[0062] Take the viscose solution obtained by the production process of conventional viscose fiber, the viscose solution indicators are: cellulose content 8.9%, NaOH content 4.7%, viscosity 52s, maturity 15ml (10% NH4CL solution). Take 600g of the ground and dispersed gingerol oil-montmorillonite inclusion suspension and 20Kg of viscose solution, and blend them evenly with a homogenizer. The mixed viscose solution is used to obtain fiber bundles through a wet spinning process. The fiber bundles are drawn, cut, desulfurized, washed, oiled, and dried to obtain gingerol cellulose fibers. Refining is not bleached, and other process controls are the same as conventional viscose fibers.

[0063] Example 3

[0064] 1. Preparation of gingerol oil-montmorillonite inclusion complex

[0065] 1) Take 10g gingerol oil into a beaker, add 20g ethanol into the beaker, and stir to dissolve thoroughly.

[0066] 2) The washed sodium-montmorillonite is prepared into a 6% suspension, 1000 g of the suspension is weighed and added to a three-necked flask, and stirred, and the fully dissolved gingerol ethanol solution is dripped into the three-necked flask.

[0067] 3) The flask was heated with a heating jacket to 80°C, and the temperature was controlled at 80±2°C. Stirring was continued for 2 hours and then cooled to room temperature to obtain a suspension of gingerol oil: sodium montmorillonite inclusion complex in a ratio of 1:6.

[0068] 4) The gingerol oil-montmorillonite inclusion complex suspension was added into a nano sand mill for grinding and dispersion to obtain a suspension with a system particle size of D90 = 1.33 μm.

[0069] 2. Preparation of gingerol cellulose fiber

[0070] Take the viscose solution obtained by the production process of conventional viscose fiber, the viscose solution indicators are: cellulose content 9.0%, NaOH content 4.7%, viscosity 56s, maturity 14ml (10% NH4CL solution). Take 600g of the ground and dispersed gingerol oil-montmorillonite inclusion suspension and 10Kg of viscose solution, and blend them evenly with a homogenizer. The mixed viscose solution is used to obtain fiber bundles through a wet spinning process. The fiber bundles are drawn, cut, desulfurized, washed, oiled, and dried to obtain gingerol cellulose fibers. Refining is not bleached, and other process controls are the same as conventional viscose fibers.

[0071] Example 4

[0072] 1. Preparation of gingerol oil-montmorillonite inclusion complex

[0073] 1) Take 10g gingerol oil into a beaker, add 20g ethanol into the beaker, and stir to dissolve thoroughly.

[0074] 2) The washed sodium-montmorillonite is prepared into a suspension with a content of 8%, 1000 g of the suspension is weighed and added to a three-necked flask, and stirred, and the fully dissolved gingerol ethanol solution is dripped into the three-necked flask.

[0075] 3) The flask was heated with a heating jacket to 80°C, and the temperature was controlled at 80±2°C. After stirring for 2 hours, the temperature was lowered to room temperature to obtain a suspension of gingerol oil: sodium montmorillonite inclusion complex in a ratio of 1:8.

[0076] 4) The gingerol oil-montmorillonite inclusion complex suspension was added into a nano sand mill for grinding and dispersion to obtain a suspension with a system particle size of D90 = 1.33 μm.

[0077] 2. Preparation of gingerol cellulose fiber

[0078] Take the viscose solution obtained by the production process of conventional viscose fiber, the viscose solution indicators are: cellulose content 8.9%, NaOH content 4.6%, viscosity 46s, maturity 16ml (10% NH4CL solution). Take 800g of the ground and dispersed gingerol oil-montmorillonite inclusion suspension and 18Kg of viscose solution, and blend them evenly with a homogenizer. The mixed viscose solution is used to obtain fiber bundles through a wet spinning process. The fiber bundles are stretched, cut, desulfurized, washed, oiled, and dried to obtain gingerol cellulose fibers. Refining is not bleached, and other process controls are the same as conventional viscose fibers.

[0079] Comparative Example

[0080] Take the viscose solution obtained by the production process of conventional viscose fiber, the indicators of the viscose solution are: cellulose content 8.9%, NaOH content 4.6%, viscosity 46s, maturity 16ml (10% NH4CL solution). Take 10g of gingerol oil and 18kg of viscose solution and blend them evenly with a homogenizer. The mixed viscose solution is used to obtain fiber bundles through a wet spinning process. The fiber bundles are stretched, cut, desulfurized, washed, oiled, and dried to obtain gingerol cellulose fibers. Refining is not bleached, and other process controls are the same as conventional viscose fibers.

[0081] The difference between this comparative example and Example 4 is that this comparative example uses gingerol oil instead of gingerol oil-montmorillonite inclusion complex.

[0082] Test Case

[0083] The main mechanical properties and gingerol content of the gingerol cellulose fibers prepared in the examples and comparative examples were tested. The results are shown in Tables 1 and Figure 2 shown.

[0084] Table 1 Comparison of gingerol cellulose fiber properties

[0085]

[0086] Note: The gingerol content extraction detection method is carried out according to the following steps:

[0087] ① Take a certain amount of gingerol cellulose fiber and make it into powder;

[0088] ② Using high-pressure and low-temperature CO2 fluid at a pressure of 8-12 MPa and a temperature of 7-20°C to extract the gingerol cellulose fiber powder to obtain the first CO2 extract;

[0089] ③ The first CO2 extract containing gingerol components in step ② is subjected to heat exchange and temperature raising to form a CO2 extract in a supercritical state;

[0090] ④ Under the conditions of pressure of 8-12MPa and temperature of 35-45°C, the supercritical CO2 extract obtained in step ③ is distilled to obtain gingerol component;

[0091] ⑤ Weigh the extracted gingerol and calculate the gingerol content in the fiber.

[0092] Through the analysis of the indicators of Examples 1-4, with the increase of the amount of gingerol oil-montmorillonite inclusion compound added, the mechanical indicators of the fiber slightly decreased, and the measured gingerol content was about 90% of the theoretical value, while in the comparative example, the gingerol oil was directly added, and the measured gingerol content was about 30% of the theoretical value. Figure 2 Thus, it can be seen that the present invention utilizes the sandwich structure of montmorillonite sheets to intercalate the dispersed gingerol oil between montmorillonite layers to form an inclusion compound, utilizes the hydrophilicity of montmorillonite to achieve uniform blending of the inclusion compound with the viscose solution to prepare gingerol cellulose fibers, and the gingerol coated with sodium-montmorillonite is continuously preserved in the cellulose fibers, thus overcoming the problem that the traditional gingerol oil is difficult to be uniformly blended with the viscose aqueous solution of cellulose, and there is no chemical reaction between the gingerol oil and cellulose, and the gingerol oil cannot achieve the problem of stable existence of gingerol in the cellulose matrix.

[0093] The above embodiments are limited to several preferred implementations of the present invention, and their descriptions are relatively specific and detailed, but they cannot be understood as limiting the scope of the present invention. It should be pointed out that for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A method for preparing gingerol cellulose fiber, characterized in that: At least the following steps are included: a. Preparation of gingerol oil-montmorillonite inclusion complex: gingerol oil was dissolved in ethanol for dispersion, and then added dropwise to the sodium montmorillonite suspension, and stirred at 78-82°C to form a gingerol oil-montmorillonite inclusion complex; b. Preparation of gingerol cellulose fiber: gingerol oil-montmorillonite inclusion complex is mixed with cellulose viscose solution, and gingerol cellulose fiber is prepared by wet spinning process.

2. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: In the step a, the mass ratio of gingerol oil to ethanol is 1:1-1:

4.

3. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: The sodium montmorillonite in step a is washed, and the washing process includes mixing the sodium montmorillonite with deionized water at a ratio of 1:20-30, washing, and filtering for several times, each time the stirring and washing time is 15-45 minutes, and the washing temperature is 78-82°C.

4. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: The concentration of the sodium montmorillonite suspension in step a is 5-10%.

5. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: In the step a, the mass ratio of gingerol oil to sodium montmorillonite is 1:5-10.

6. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: After the gingerol oil-montmorillonite inclusion complex in step a is reacted, it is further ground and dispersed, and the particle size D90 of the system is ≤2 μm.

7. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: In the step b, the mass ratio of sodium montmorillonite to cellulose is 1:20-30.

8. The method for preparing gingerol cellulose fiber according to claim 1, characterized in that: The following steps are involved: a Preparation of gingerol oil-montmorillonite inclusion complex: 1) Mix gingerol oil and ethanol in a mass ratio of 1:1-1:4; 2) Mix sodium montmorillonite and deionized water at a ratio of 1:20-30, wash and filter for 3 times, each time for 30 minutes, and the washing temperature is controlled at 78-82°C; 3) adding deionized water to the washed sodium montmorillonite to prepare a 5-10% suspension; 4) Slowly drop gingerol oil dissolved in ethanol into the stirred and dispersed sodium montmorillonite suspension, the amount of drop is controlled according to the mass ratio of gingerol oil: sodium montmorillonite = 1:5-10, the temperature is controlled at 78-82°C, and the stirring is continued for 1-3h and then cooled to room temperature; 5) adding the gingerol oil-montmorillonite inclusion complex suspension into a nano sand mill for grinding and dispersion, and stopping grinding when the system particle size D90 is ≤2 μm, and packaging for standby use to obtain the gingerol oil-montmorillonite inclusion complex; b Preparation of gingerol cellulose fiber: 1) Preparation of gingerol oil-montmorillonite inclusion complex and viscose blend solution The same as the conventional viscose fiber production process, the cellulose viscose solution is prepared through pulp impregnation, pressing, crushing, aging, yellowing, dissolving, filtering, and degassing steps, the ground gingerol oil-montmorillonite inclusion compound is added to the viscose solution, homogenized and mixed evenly, and the amount of inclusion compound added is controlled by the mass ratio of sodium montmorillonite: cellulose = 1:20-30; 2) Spinning and post-treatment of gingerol cellulose fibers The gingerol oil-montmorillonite inclusion compound and viscose mixed solution are used to obtain fiber bundles through a wet spinning process, and the fiber bundles are stretched, cut, desulfurized, washed, oiled and dried to obtain gingerol cellulose fibers.

9. Gingerol cellulose fiber obtained by the preparation method according to any one of claims 1 to 8.

10. The gingerol cellulose fiber according to claim 9, characterized in that: The mass percentage of gingerol in the gingerol cellulose fiber is ≥0.35%, and the content is detected by an extraction detection method.

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