CN114808180B

CN114808180B - Bamboo charcoal fiber manufacturing method

Info

Publication number: CN114808180B
Application number: CN202210401645.0A
Authority: CN
Inventors: 张雪飞
Original assignee: Inner Mongolia Mengneng Environmental Protection Technology Co ltd
Current assignee: Inner Mongolia Mengneng Environmental Protection Technology Co ltd
Priority date: 2022-04-18
Filing date: 2022-04-18
Publication date: 2023-11-28
Anticipated expiration: 2042-04-18
Also published as: CN114808180A

Abstract

The invention discloses a method for manufacturing bamboo charcoal fibers, and relates to the field of textile materials. The preparation method comprises micronizing bamboo charcoal by grinding technology, mixing the bamboo charcoal micropowder with carrier, coupling agent, surfactant, dispersant and dandelion flavone, and melt mixing and spinning the obtained bamboo charcoal masterbatch with carrier slice to obtain bamboo charcoal fiber with good mechanical properties, moisture regain and lower friction coefficient; the invention also provides a modification method of the dispersing agent, which adopts oridonin to graft and modify the polyethylene wax, thereby further improving the dispersion performance of the bamboo charcoal micro powder in the preparation process of the bamboo charcoal master batch.

Description

Bamboo charcoal fiber manufacturing method

Technical Field

The invention belongs to the field of textile materials, and particularly relates to a method for manufacturing bamboo charcoal fibers.

Background

The bamboo resources in China are rich, the area of the bamboo forest and the bamboo wood yield account for about 1/3 of the world, and the first world is called as "bamboo kingdom". However, the existing bamboo products are mainly direct processed products with low technical content and low added value and comprehensive utilization rate, the development of bamboo charcoal textiles can improve the utilization rate of bamboo from 40% to over 95%, and the bamboo can be increased by 5-10 times, so that the method plays a vital role in solving the problem that the export quantity is large but the economic benefit is not very good due to export primary processed bamboo products in China. The bamboo charcoal mainly comprises elements such as carbon, hydrogen, oxygen and the like, has hard texture, is fine and porous, has strong adsorption capacity, has the adsorption capacity which is more than 10 times that of charcoal with the same volume, and contains mineral substances which are more than 5 times that of charcoal with the same volume, so that the bamboo charcoal has good deodorizing, antiseptic and odor adsorption functions. The bamboo charcoal can adsorb and neutralize acidic substances contained in sweat, so as to achieve the effect of whitening skin. And the bamboo charcoal is also a good far infrared and anion emitting material. It not only has natural and environmental protection characteristics, but also has a plurality of functions such as far infrared rays, anions, heat accumulation, warmth retention and the like, and is suitable for underwear. The bamboo charcoal has permanent function and is not affected by the washing times. The nanometer bamboo charcoal micropowder also has good antibacterial and bactericidal effects.

Along with the change of the living mode and living environment of modern people, people more and more keep on a natural and healthy living mode, the birth of the bamboo charcoal fiber meets the pursuit of people, the bamboo charcoal fiber is internationally praised as a '21 st century environment-friendly new guard', the excellent performance which is incomparable with the traditional fiber is fully utilized, and the development of the functional bamboo charcoal fiber gradually becomes a main stream product of the functional health care textile market. The invention prepares bamboo charcoal micropowder by grinding technology, then prepares bamboo charcoal master batch by mixing the bamboo charcoal micropowder with auxiliary agent, and then carries out spinning after melting and mixing the bamboo charcoal master batch and carrier slices; in addition, in the preparation process, oridonin is adopted to carry out grafting modification on the dispersion polyethylene wax, and the prepared bamboo charcoal fiber has good performance while being environment-friendly and safe.

Disclosure of Invention

The invention aims to provide a method for manufacturing bamboo charcoal fiber, which has good mechanical properties, moisture regain and lower friction coefficient.

The technical scheme adopted by the invention for achieving the purpose is as follows:

a method for manufacturing bamboo charcoal fiber, comprising:

(1) Grinding bamboo charcoal into nanometer bamboo charcoal micropowder;

(2) Mixing the bamboo charcoal micropowder with carrier, coupling agent, surfactant, dispersant and dandelion flavone to obtain bamboo charcoal master batch;

(3) And mixing the bamboo charcoal master batch with a carrier under stirring, and performing melt spinning to obtain the bamboo charcoal fiber.

The invention provides a method for manufacturing bamboo charcoal fiber, which comprises the steps of grinding bamboo charcoal to obtain bamboo charcoal micropowder with the particle size of 55-70nm, adding a carrier, a silane coupling agent, a surfactant, a dispersing agent and dandelion flavone into the bamboo charcoal micropowder, mixing to obtain bamboo charcoal master batch, adding the bamboo charcoal master batch into a carrier slice, and carrying out melt mixing spinning to obtain the bamboo charcoal fiber with good mechanical properties, moisture regain and lower friction coefficient. The invention provides a thought for the preparation of the bamboo charcoal in the aspect of textiles and lays a scientific theoretical foundation for the application of the bamboo charcoal fiber in the aspect of functional textiles.

In some embodiments of the present invention, the particle size of the bamboo charcoal micropowder in step (1) is: 55-70nm.

In some embodiments of the invention, the friction coefficient of the bamboo charcoal fiber is less than or equal to 0.295; more preferably, the friction coefficient of the bamboo charcoal fiber is less than or equal to 0.152.

In some embodiments of the invention, the support in step (1) and step (2) comprises polyester chips.

In some embodiments of the present invention, in the step (2), the mass ratio of the bamboo charcoal micro powder to the coupling agent is: 1:0.03-0.05; the mass ratio of the bamboo charcoal micro powder to the surfactant is as follows: 1:0.02-0.03; the mass ratio of the bamboo charcoal micro powder to the dispersing agent is as follows: 1:0.5-0.8.

In some embodiments of the invention, the coupling agent comprises a silane coupling agent.

In some embodiments of the invention, the dispersant comprises polyethylene wax.

In some embodiments of the invention, the surfactant comprises a fatty acid glyceride.

In some embodiments of the present invention, the mass ratio of the carrier to the bamboo charcoal micropowder in step (2) is: 1:0.6-0.75.

In some embodiments of the present invention, the mass ratio of the bamboo charcoal micropowder to dandelion flavone in the step (2) is: 1:0.03-0.05.

In some embodiments of the invention, the mixing conditions in step (2) are: the temperature is 270-275 ℃, the rotating speed is 300-350r/min, the pressure is 12-15MPa, and the time is 5-8min.

In some embodiments of the invention, the amount of the bamboo charcoal master batch in the step (3) is 15-30wt% of the amount of the carrier.

In some embodiments of the present invention, the melt spinning temperature in step (3) is: 267-272 ℃.

More preferably, the invention uses modified polyethylene wax to replace polyethylene wax in the bamboo charcoal fiber manufacturing process.

The invention also provides a preparation method of the modified polyethylene wax, which comprises the following steps: the modified polyethylene wax is prepared by grafting modification of the polyethylene wax by oridonin.

The invention discloses a preparation method of modified polyethylene wax, which takes dibenzoyl peroxide as an initiator in the preparation process, adopts oridonin to carry out grafting modification on the polyethylene wax, and the prepared modified polyethylene wax is used as a dispersing agent in the preparation process of bamboo charcoal master batch, and is possibly beneficial to the preparation of bamboo charcoal fibers because the oridonin changes the polarity of the polyethylene wax, so that the modified polyethylene wax improves the dispersion performance of bamboo charcoal micro powder in the master batch.

Specifically, the preparation method of the modified polyethylene wax comprises the following steps:

adding toluene into polyethylene wax, heating to 110-120 ℃, stirring to dissolve, slowly adding oridonin and dibenzoyl peroxide, reacting for 1-1.5h at 185-195 ℃, pouring out the product while the product is hot, cooling and solidifying, and extracting for 5-7h in a Soxhlet extractor by using acetone to obtain the modified polyethylene wax.

In some embodiments of the present invention, the mass-to-volume ratio of the polyethylene wax to toluene is: 1g, 2.5-4mL; the mass ratio of the polyethylene wax to the oridonin is as follows: 1:0.1-0.15; the mass ratio of the polyethylene wax to the dibenzoyl peroxide is as follows: 1:0.015-0.03.

The invention also discloses the application of the bamboo charcoal fiber prepared by the preparation method in preparing functional textiles.

The beneficial effects of the invention include:

the invention has obtained a bamboo charcoal fiber manufacturing approach, adopt the grinding to make the bamboo charcoal micropowder with particle diameter of 55-70nm, then mix the bamboo charcoal micropowder with carrier, silane coupling agent, surfactant, dispersant, dandelion flavone, make the master batch of bamboo charcoal, mix the master batch of bamboo charcoal with carrier and spin in fusion, the bamboo charcoal fiber obtained has good mechanical properties, moisture regain and lower coefficient of friction; the invention also takes dibenzoyl peroxide as an initiator to carry out grafting modification on oridonin and polyethylene wax; the prepared modified polyethylene wax is used as a dispersing agent for preparing bamboo charcoal master batch; so that the bamboo charcoal micropowder has good dispersion property in the bamboo charcoal master batch.

Therefore, the invention provides a method for manufacturing the bamboo charcoal fiber, and the bamboo charcoal fiber prepared by the method has good mechanical property, moisture regain and lower friction coefficient.

Drawings

FIG. 1 shows the results of infrared spectrum test of the modified polyethylene wax and polyethylene wax prepared in example 4.

Detailed Description

The technical scheme of the invention is further described in detail below with reference to the specific embodiments and the attached drawings:

the silane coupling agent KH550 used in the embodiment of the invention is purchased from Shandong Ring chemical Co., ltd;

the glycerol laurate used in the embodiment of the invention is purchased from Jiaxing middle-hong environmental protection science and technology Co., ltd;

the polyethylene wax used in the embodiment of the invention is purchased from Shanghai Yiba chemical raw materials Co., ltd;

the dandelion flavone used in the embodiment of the invention is purchased from Shaanxi Guanyin biotechnology Co., ltd;

oridonin used in the examples of the present invention was purchased from Shanxi Chen Biotechnology Co.

Example 1:

a method for manufacturing bamboo charcoal fiber comprises the following steps:

(1) Grinding bamboo charcoal into nanometer bamboo charcoal micropowder with particle diameter of 60nm.

(2) Adding polyester chips (the mass ratio of the polyester chips to the bamboo charcoal micro powder is 1:0.6), a silane coupling agent KH550, laurin, polyethylene wax and dandelion flavone into the bamboo charcoal micro powder for mixing, wherein the mixing conditions are as follows: the temperature is 270 ℃, the rotating speed is 300r/min, the pressure is 12MPa, and the time is 5min, so that the bamboo charcoal master batch is prepared;

(3) Adding the bamboo charcoal master batch into a polyester chip (the dosage of the bamboo charcoal master batch is 25wt% of the dosage of the polyester chip), stirring and mixing, and carrying out melt spinning at 270 ℃ to obtain bamboo charcoal fibers;

wherein, the mass ratio of the bamboo charcoal micro powder to the silane coupling agent KH550 is as follows: 1:0.03; the mass ratio of the bamboo charcoal micro powder to the laurin is as follows: 1:0.02; the mass ratio of the bamboo charcoal micro powder to the polyethylene wax is as follows: 1:0.5; the mass ratio of the bamboo charcoal micro powder to dandelion flavone is as follows: 1:0.03.

Example 2:

the difference between the method for producing bamboo charcoal fiber and example 1 is that: the mass ratio of the bamboo charcoal micro powder to the silane coupling agent KH550 is as follows: 1:0.05; the mass ratio of the bamboo charcoal micro powder to the laurin is as follows: 1:0.03; the mass ratio of the bamboo charcoal micro powder to the polyethylene wax is as follows: 1:0.8; the mass ratio of the bamboo charcoal micro powder to dandelion flavone is as follows: 1:0.05.

Example 3:

the difference between the method for producing bamboo charcoal fiber and example 1 is that: the mass ratio of the bamboo charcoal micro powder to the silane coupling agent KH550 is as follows: 1:0.04; the mass ratio of the bamboo charcoal micro powder to the surfactant is as follows: 1:0.025; the mass ratio of the bamboo charcoal micro powder to the polyethylene wax is as follows: 1:0.6; the mass ratio of the bamboo charcoal micro powder to dandelion flavone is as follows: 1:0.04.

Example 4:

the difference between the method for producing bamboo charcoal fiber and example 1 is that: and adopting modified polyethylene wax to replace polyethylene wax.

The preparation method of the modified polyethylene wax comprises the following steps:

adding toluene into polyethylene wax, heating to 110 ℃, stirring to dissolve, slowly adding oridonin and dibenzoyl peroxide, reacting for 1h at 185 ℃, pouring out the product while the product is hot, cooling and solidifying, and extracting for 5h in a Soxhlet extractor by using acetone to obtain modified polyethylene wax; wherein the mass volume ratio of the polyethylene wax to the toluene is as follows: 1g:2.5ml; the mass ratio of the polyethylene wax to the oridonin is as follows: 1:0.1; the mass ratio of the polyethylene wax to the dibenzoyl peroxide is as follows: 1:0.015.

Example 5:

the difference between the method for producing bamboo charcoal fiber and example 4 is that: the mass volume ratio of the polyethylene wax to the toluene is as follows: 1g:4mL; the mass ratio of the polyethylene wax to the oridonin is as follows: 1:0.15; the mass ratio of the polyethylene wax to the dibenzoyl peroxide is as follows: 1:0.03.

Example 6:

the difference between the method for producing bamboo charcoal fiber and example 4 is that: the mass volume ratio of the polyethylene wax to the toluene is as follows: 1g:3ml; the mass ratio of the polyethylene wax to the oridonin is as follows: 1:0.13; the mass ratio of the polyethylene wax to the dibenzoyl peroxide is as follows: 1:0.02.

Example 7:

the difference between the method for producing bamboo charcoal fiber and example 4 is that: herba Taraxaci flavone is not added.

Example 8:

the difference between the method for producing bamboo charcoal fiber and example 1 is that: herba Taraxaci flavone is not added.

Test example 1:

infrared spectroscopy testing

The sample is tested and analyzed by adopting a Fourier infrared spectrometer and taking pure potassium bromide as a background, and the resolution is 2cm ^-1 The scanning times are 20 times, and the scanning range is 4000-400 cm ^-1 。

The modified polyethylene wax prepared in example 4 and the polyethylene wax were subjected to the above-described test, and the results are shown in fig. 1. As can be seen from FIG. 1, in the infrared spectrum of the modified polyethylene wax, 1635cm ^-1 At which there is a characteristic absorption peak of c=o; at 1134cm ^-1 Characteristic absorption peaks of C-O bonds exist at the positions; indicating that oridonin participates in the formation reaction of the modified polyethylene wax.

Test example 2:

dispersion performance test

And observing the particle size of the bamboo charcoal micropowder in the dispersing agent by using a DB-525 laser particle size analyzer, and analyzing the dispersing performance by the particle size.

TABLE 1 average particle size test results of bamboo charcoal micropowder in dispersant

Grouping	Average particle diameter/nm
		Modified polyethylene wax	60-75
Polyethylene wax	80-100

The above-mentioned test was conducted on the particle size of the bamboo charcoal fine powder in the modified polyethylene wax prepared in example 4 and the polyethylene wax, and the results are shown in table 1. From table 1, the particle size of the bamboo charcoal micropowder in the modified polyethylene wax is obviously smaller than that in the polyethylene wax, which shows that the modified polyethylene wax prepared from oridonin has good dispersion performance, probably because oridonin modifies the polarity of the modified polyethylene wax, and the polarity of the dispersing agent is closely related to the dispersion effect of the modified polyethylene wax.

Test example 3:

mechanical property test

Testing the mechanical properties of the bamboo charcoal fiber sample by adopting an YG001 type electronic fiber strength tester; the experimental group is as follows: example 1 is designated S1; example 2 is designated S2; example 3 is designated S3; example 4 is designated S4; example 5 is designated S5; example 6 is designated S6; example 7 is designated S7; example 8 is designated S8; the parameters of the brute force instrument are set as follows: the stretching distance was set at 20mm, the stretching speed was adjusted to 20mm/min, and the constant-speed stretching was maintained by using a pre-tension of 0.088cN/dtex, and each sample was tested 50 times, and an average value was obtained.

TABLE 2 results of breaking Strength test of different bamboo charcoal fiber samples

Grouping of samples	Breaking strength/CN ∙ dtex ^-1
		S1	5.08
S2	5.16
		S3	5.11
S4	5.29
		S5	5.33
S6	5.30
		S7	4.32
S8	4.15

The above-mentioned test was performed on the bamboo charcoal fibers prepared in examples 1 to 8, and the results are shown in table 2. As is clear from table 2, the increase in breaking strength of example 4 compared with example 1 and example 7 compared with example 8 indicates that the use of the modified polyethylene wax has an effect of improving the breaking strength of the bamboo charcoal fiber; compared with example 7 and example 1 and example 8, the breaking strength of example 4 is obviously increased, which indicates that the addition of dandelion flavone ensures that the bamboo charcoal fiber has higher breaking strength and good mechanical properties.

Test example 4:

test of moisture regain

The bamboo charcoal fiber sample is placed under the condition of standard atmosphere (the temperature is 20+/-2 ℃ and the relative humidity is 65% +/-2%) for balancing for 48 hours, weighed, then placed into an oven, the temperature is set to be 105+/-3 ℃, timing is started after the temperature of the oven is raised to the set temperature, the oven is opened after baking for 1.5 hours, and the oven is balanced for 10 minutes and then weighed; experimental grouping conditions are the same as in experimental example 3; the moisture regain is the percentage of the weight of moisture contained in the textile material to the dry weight of the textile material and is calculated as follows:

R/%=[(m0-m1)/m1]×100%

wherein R is the moisture regain,%; m0 is the mass of the sample before baking, g; m1 is the mass of the sample after drying and g.

TABLE 3 results of moisture regain test of different bamboo charcoal fiber samples

Grouping of samples	Moisture regain/%
		S1	0.95
S2	0.98
		S3	0.94
S4	1.23
		S5	1.26
S6	1.25
		S7	1.21
S8	0.92

The above-mentioned test was performed on the bamboo charcoal fibers prepared in examples 1 to 8, and the results are shown in table 3. As can be seen from table 3, the moisture regain of example 4 is significantly increased compared with examples 1 and 7 and 8, which indicates that the use of the modified polyethylene wax has an effect of improving the moisture regain of the bamboo charcoal fiber, probably because the modified polyethylene wax disperses the bamboo charcoal micropowder more uniformly, thereby improving the moisture regain of the bamboo charcoal fiber; compared with example 7 and example 1 and example 8, the moisture regain of example 4 is not greatly different, which shows that the addition of dandelion flavone has no obvious effect on the moisture regain of the bamboo charcoal fiber.

Test example 5:

testing of coefficient of friction

The test is carried out on the bamboo charcoal fiber sample by adopting a Y151 type fiber friction factor meter, and the experimental grouping condition is the same as that of the experimental example 3; the fiber roll speed was set at 30r/min, each set of samples was tested 3 times and averaged.

TABLE 4 results of Friction coefficient test of different bamboo charcoal fiber samples

Grouping of samples	Coefficient of friction
		S1	0.233
S2	0.229
		S3	0.230
S4	0.147
		S5	0.152
S6	0.149
		S7	0.214
S8	0.295

The above-mentioned test was performed on the bamboo charcoal fibers prepared in examples 1 to 8, and the results are shown in table 4. As can be seen from table 4, the friction coefficient of example 4 is significantly lower than that of example 1 and example 7 compared with that of example 8, which indicates that the use of the modified polyethylene wax reduces the friction coefficient of the bamboo charcoal fiber; compared with example 7 and example 1 and example 8, the friction coefficient of example 4 is reduced, which indicates that the addition of dandelion flavone makes the bamboo charcoal fiber have lower friction coefficient; the reason is probably that the friction coefficient is also reduced because the fibers tend to be full due to the addition of the dandelion flavone which is a small molecular substance.

The conventional technology in the above embodiments is known to those skilled in the art, and thus is not described in detail herein.

The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims

1. A method for manufacturing bamboo charcoal fiber, comprising:

(1) Grinding bamboo charcoal into nanometer bamboo charcoal micropowder;

(3) Mixing bamboo charcoal master batch with a carrier under stirring, and performing melt spinning to obtain bamboo charcoal fiber;

the carrier comprises polyester chips;

in the step (2), the mass ratio of the bamboo charcoal micro powder to the coupling agent is as follows: 1:0.03-0.05; the mass ratio of the bamboo charcoal micro powder to the surfactant is as follows: 1:0.02-0.03; the mass ratio of the bamboo charcoal micro powder to the dispersing agent is as follows: 1:0.5-0.8; the mass ratio of the bamboo charcoal micro powder to dandelion flavone is as follows: 1:0.03-0.05;

the dispersing agent is modified polyethylene wax;

2. The method for producing bamboo charcoal fiber according to claim 1, wherein: the particle size of the bamboo charcoal micropowder is as follows: 55-70nm.

3. The method for producing bamboo charcoal fiber according to claim 1, wherein: the friction coefficient of the bamboo charcoal fiber is less than or equal to 0.295.

4. The method for producing bamboo charcoal fiber according to claim 1, wherein: the coupling agent is a silane coupling agent.

5. The method for producing bamboo charcoal fiber according to claim 1, wherein: the surfactant is fatty glyceride.

6. The method for producing bamboo charcoal fiber according to claim 1, wherein: the mixing conditions are as follows: the temperature is 270-275 ℃, the rotating speed is 300-350r/min, the pressure is 12-15MPa, and the time is 5-8min.

7. Use of the bamboo charcoal fiber produced by the production method of any one of claims 1 to 6 for producing functional textiles.