TW201443086A - Viscose composition and preparing method thereof and polysacharide composite material - Google Patents

Abstract

A preparing method of viscose composition is provided. In the preparing method of viscose composition, a polysaccharide material is provided, wherein the polysaccharide material includes a cellulose and a chitin. The polysaccharide material are mixed with an ionic liquid to form a polysaccharide solution. A dilutant is added to the polysaccharide solution to form a viscose composition.

Description

Mucus composition, preparation method thereof and polysaccharide composite material

The invention relates to a mucus composition, a preparation method thereof and a polysaccharide composite material, and particularly relates to a low viscosity mucus composition, a preparation method thereof and a polysaccharide composite material.

In recent years, scientists have actively developed the production of recycled fibers to replace the consumption of natural fibers by dissolving existing polymer materials. Recycled fibers can be used in a wide variety of industries, such as home textiles, optical films, flexible electronic displays, cosmetics, medical drugs and food additives. In the natural world, the content of cellulose ranks first, so cellulose is currently the main raw material for recycled fiber.

In addition, in the process of reclaiming fibers, various chemical or physical methods are generally used to enable the regenerated fibers to have various functions to meet market demands, such as gas permeability, moisture absorption, easy dyeing, antistatic, antibacterial, and the like.

Chitin is the second largest natural polymer material second only to cellulose, and chitin has good biocompatibility, hygroscopicity, and superior antibacterial and deodorant properties. Features. At present, chitin is used in the prior art to prepare regenerated fibers. However, chitin fibers are hard and brittle when dried, so application is limited. Therefore, how to prepare a low-cost and functional cellulose/chitin composite material will be the current active research direction.

The invention provides a preparation method of a mucus composition, which can reduce the amount of the ionic liquid and obtain a mucus composition with reduced viscosity.

The present invention further provides a mucus composition which has low viscosity and good processability.

The present invention further provides a polysaccharide composite material formed from the mucus composition provided by the present invention.

The present invention provides a method for preparing a mucus composition, the method comprising the following steps. A polysaccharide material is provided, wherein the polysaccharide material comprises cellulose and chitin. The polysaccharide material is mixed with an ionic liquid to form a polysaccharide solution. A diluent is added to the polysaccharide solution to form a mucus composition.

The present invention further provides a mucus composition comprising a polysaccharide material, an ionic liquid, and a diluent, wherein the viscosity of the mucus composition is from 1000 cPs to 200,000 cPs. The polysaccharide material includes cellulose and chitin, wherein the ratio of cellulose to chitin is 9:1 to 1:9 by weight, and the content of the polysaccharide material is 1 wt% based on the total weight of the mucus composition. % to 25 wt%. The polysaccharide material is dissolved in the ionic liquid. Depending on the total weight of the mucus composition, both the ionic liquid and the diluent are added. The total content is from 75 wt% to 99 wt%. Further, the ratio of the ionic liquid to the diluent is from 9:1 to 1:1 by weight.

The invention further proposes a polysaccharide composite material comprising cellulose and chitin, wherein the ratio of cellulose to chitin is from 9:1 to 1:9 by weight.

Based on the above, the mucus composition proposed by the embodiment of the present invention, the preparation method thereof, and the polysaccharide composite material can effectively reduce the viscosity of the mucus composition by further dissolving the polysaccharide material by using the ionic liquid, and then increasing the viscosity of the mucus composition. The processability of the mucus composition.

The above described features and advantages of the invention will be apparent from the following description.

S10~S14‧‧‧Steps

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the preparation of a mucus composition according to an embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the preparation of a mucus composition according to an embodiment of the present invention. Referring to FIG. 1, step S10 of FIG. 1 is performed to provide a polysaccharide material, wherein the polysaccharide material comprises cellulose and chitin. In the present embodiment, the ratio of the above cellulose to chitin is, for example, 9:1 to 1:9 by weight. In one embodiment, the ratio of cellulose to chitin is, for example, 9:1 to 1:1 by weight. In another reality In the examples, the ratio of the above cellulose to chitin is, for example, 9:1, 3:1, and 1:1 by weight.

Next, step S12 of Fig. 1 is carried out to mix the polysaccharide material with the ionic liquid to form a polysaccharide solution. In the present embodiment, the ionic liquid is composed, for example, of a cation and an anion, and the above cation includes a structure as shown in Formula 1:

Wherein R ₁ to R ₅ are H or a hydrocarbon group having 1 to 8 carbon atoms; and the above anion is, for example, one selected from the group consisting of Cl ^- , Br ^- , I ^- , CH ₃ COO ^- and HCOO ^- .

Generally, a polysaccharide material generally has a plurality of hydrogen bond donors and a hydrogen bond acceptor in its molecular structure. For example, in the polysaccharide material of the present embodiment, the hydrogen bond provider is a hydrogen atom in the hydroxyl group, and the hydrogen bond acceptor is an oxygen atom in the hydroxyl group. As a result, the polysaccharide material not only has hydrogen bonds widely inside the molecule, but also has a certain degree of intramolecular polarity, and the molecules and molecules of the polysaccharide material are also prone to hydrogen bonds, which will make the polysaccharide materials in the conventional It is difficult to dissolve in solvents such as water and most organic solvents.

In the present embodiment, the cations and anions in the ionic liquid can interact with oxygen atoms and hydrogen atoms in the polysaccharide material, thereby breaking the hydrogen bonds between the molecules of the polysaccharide material, thereby fully dissolving the polysaccharides. Material and form polysaccharide Solution.

Further, in one embodiment, the ionic liquid is, for example, 1-ethyl-3-methylimidazolium acetate (EMIMOAc). In particular, an ionic liquid having an anion of CH ₃ COO ⁻ (1-ethyl-3-methylimidazolium acetate as described above) and an anion having an anion of an ionic liquid of another species (for example, Cl ⁻ ) are The ionic liquid of CH ₃ COO ^- can dissolve the same amount of polysaccharide material at a lower temperature, thereby reducing the energy used in dissolution.

Further, in the present embodiment, the total solid content of the polysaccharide solution is, for example, 1% to 25%. In one embodiment, the total solids content of the polysaccharide solution is, for example, from 5% to 10%. In another embodiment, the total solids content of the polysaccharide solution is, for example, 5%.

Next, step S14 of Fig. 1 is carried out, and a diluent is added to the polysaccharide solution to form the slime composition. In the present embodiment, the ratio of the ionic liquid to the diluent is, for example, 9:1 to 1:1 by weight. In one embodiment, the ratio of ionic liquid to diluent is, for example, from 5:1 to 1:1 by weight. In another embodiment, the ratio of ionic liquid to diluent is, for example, 5:1 by weight. Further, in the present embodiment, the diluent is, for example, dimethyl sulfoxide (DMSO), dimethylformamide (DMF) or N-methylpyrrolidone (1-Methyl-2-pyrrolidone, NMP). In one embodiment, the diluent is, for example, dimethyl hydrazine. Further, in the present embodiment, the viscosity of the slime composition is, for example, 1000 cPs to 200,000 cPs.

In particular, the present invention uses an ionic liquid together with a diluent as a solvent, wherein the polysaccharide material is mainly dissolved in the ionic liquid and then added to the diluent. The release agent is diluted. In this way, not only the viscosity of the mucus composition can be lowered, but also the use of the diluent can reduce the amount of the ionic liquid, thereby reducing the cost of using the solvent. In general, the viscosity of the mucus composition is an important factor affecting the processability for subsequent processing of the mucus composition (described below). For example, when the mucus composition is subjected to a coating process or an extrusion process, the viscosity of the mucus composition is usually controlled in the range of 2000 cps to 200,000 cps, preferably 10,000 cps to 100,000 cps. In the range.

Further, by adjusting the concentration of the diluent in the mucus composition, the viscosity of the mucus composition can be further changed, so that the mucus composition of the present invention can be applied to more fields. For example, if a rubber type gel is required, the amount of the diluent can be reduced and the amount of the polysaccharide material can be relatively increased; in addition, if a lubricant having a viscosity is prepared, the amount of the diluent can be increased. To reduce the viscosity of the mucus composition.

Further, in the present invention, although a diluent is added as a solvent in addition to an ionic liquid as a solvent, the present invention can effectively recover a relatively expensive ionic liquid. Hereinafter, an example in which 1-ethyl-3-methylimidazolium acetate is used as the ionic liquid and dimethylhydrazine is used as the diluent will be described, but the present invention is not limited thereto. In this case, since 1-ethyl-3-methylimidazolium acetate and dimethyl hydrazine are mutually soluble, and 1-ethyl-3-methylimidazolium acetate is also miscible with water, When the solvent is recovered, the dimethyl hydrazine can be removed and the water removed first. The detailed method is as follows. First, dimethyl hydrazine was extracted using diethyl ether. After that, use 1-ethyl-3-methylimidazolium acetate by distillation or lyophilization. The water is removed, and the purpose of recovering 1-ethyl-3-methylimidazolium acetate is effectively achieved.

Therefore, the preparation of the mucus composition of the present embodiment can be completed by performing all of the above steps (S10 to S14).

In other words, the mucus composition proposed in the present embodiment includes a polysaccharide material, an ionic liquid, and a diluent, wherein the viscosity of the mucus composition is, for example, 1000 cPs to 200,000 cPs. In one embodiment, the viscosity of the mucus composition is, for example, 46999 cPs to 55233 cPs.

Further, in the mucus composition of the present embodiment, the content of the polysaccharide material is, for example, 1 wt% to 25 wt% based on the total weight of the mucus composition, and the total content of both the ionic liquid and the diluent is, for example, It is 75 wt% to 99 wt%. In one embodiment, the content of the polysaccharide material is, for example, 1 wt% to 20 wt%, based on the total weight of the mucus composition, and the total content of both the ionic liquid and the diluent is, for example, 80 wt% to 99. Wt%.

It is also mentioned that the mucus composition obtained through all the above steps (S10 to S14) can be further processed to form a polysaccharide composite material. In the present embodiment, the polysaccharide composite material can be used as a film, and the production steps are as follows. First, the mucus composition is applied onto a substrate, and the mucus composition is washed with a non-solvent to form a mucus composition. In this embodiment, the substrate is, for example, a glass substrate or other suitable substrate. The non-solvent is, for example, water, methanol, ethanol or propanol. Next, the mucus composition is subjected to a drying process to form a polysaccharide composite. However, the invention is not limited thereto. In other embodiments, the polysaccharide composite can be used as a fiber.

In this embodiment, the polysaccharide composite material comprises cellulose and chitin, wherein the ratio of cellulose to chitin is from 9:1 to 1:9 by weight. In one embodiment, the ratio of cellulose to chitin in the polysaccharide composite is, for example, from 9:1 to 1:1 by weight. In addition, the polysaccharide composite material of the present embodiment can be applied to related industries such as textiles, food processing, and biomedical materials.

Hereinafter, the above embodiments will be described in detail by means of several experimental examples. Preparation and characteristics of mucus composition. However, the following experimental examples are not intended to limit the invention.

Experimental example one

In order to demonstrate that the present invention can prepare a mucus composition comprising a composite of cellulose and chitin, and each mucilage composition has excellent viscosity, the following experimental examples are particularly preferred.

Preparation of mucus composition Example 1

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 9:1 by weight. Next, 1-ethyl-3-methylimidazolium acetate as an ionic liquid was mixed with cellulose and chitin at 60 ° C for 8 hours to dissolve 1-ethyl-3-methylimidazolium acetate. Cellulose and chitin form a polysaccharide solution with a total solid content of 5%. Thereafter, dimethyl hydrazine as a diluent is added to form a mucilage composition, wherein the dimethyl hydrazine is added in a ratio by weight to the ratio of 1-ethyl-3-methylimidazolium acetate: 5.

Example 2

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 3:1 by weight. Next, 1-ethyl-3-methylimidazolium acetate as an ionic liquid was mixed with cellulose and chitin at 60 ° C for 8 hours to dissolve 1-ethyl-3-methylimidazolium acetate. Cellulose and chitin form a polysaccharide solution with a total solid content of 5%. Thereafter, dimethyl hydrazine as a diluent is added to form a mucilage composition, wherein the dimethyl hydrazine is added in a ratio by weight to the ratio of 1-ethyl-3-methylimidazolium acetate: 5.

Example 3

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 1:1 by weight. Next, 1-ethyl-3-methylimidazolium acetate as an ionic liquid was mixed with cellulose and chitin at 60 ° C for 8 hours to dissolve 1-ethyl-3-methylimidazolium acetate. Cellulose and chitin form a polysaccharide solution with a total solid content of 5%. Thereafter, dimethyl hydrazine as a diluent is added to form a mucilage composition, wherein the dimethyl hydrazine is added in a ratio by weight to the ratio of 1-ethyl-3-methylimidazolium acetate: 5.

Comparative example 1

First, cellulose as a polysaccharide material is provided. Next, 1-ethyl-3-methylimidazolium acetate as an ionic liquid was mixed with cellulose at 60 ° C for 8 hours to dissolve the cellulose in 1-ethyl-3-methylimidazolium acetate. A polysaccharide solution having a total solid content of 5% was formed. Thereafter, dimethyl hydrazine is added as a diluent to form a slime composition, wherein the dimethyl hydrazine is added in a ratio by weight to the ratio of 1-ethyl-3-methylimidazolium acetate: 5.

Viscosity measurement

Next, the mucus compositions of Examples 1 to 3 and the mucus composition of Comparative Example 1 were subjected to viscosity measurement, and the respective measurement results are shown in Table 1. The instruments used and the measurement parameters are as follows: Instrument: Viscometer (Model: DV-II+Pro, manufactured by Brookfield). Torque value: 90%.

As is apparent from Table 1, the viscosity of the mucus composition of Examples 1 to 3 was lower than that of Comparative Example 1. In addition, when the proportion of chitin is higher and higher, the viscosity tends to decrease gradually. The cause of this phenomenon is presumably because the molecular weight of chitin is lower than the molecular weight of cellulose, so when the proportion of chitin is increased, the viscosity tends to decrease.

Experimental example 2

In this experimental example, the mucus composition of Example 1 was compared with a polysaccharide solution obtained using a different solvent, and a viscosity measurement was performed.

Preparation of mucus composition Comparative example 2

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 9:1 by weight. Then, at 60 ° C, it will act as Ionic liquid 1-ethyl-3-methylimidazolium acetate and dimethyl hydrazine (cosolvent) were mixed with cellulose and chitin for 8 hours to make 1-ethyl-3-methylimidazolium acetate The salt dissolves cellulose and chitin to form a polysaccharide solution having a total solid content of 5%, wherein the dimethyl hydrazine is added in a ratio by weight to the ratio of 1-ethyl-3-methylimidazolium acetate: 5.

Comparative example 3

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 9:1 by weight. Next, 1-ethyl-3-methylimidazolium acetate as an ionic liquid was mixed with cellulose and chitin at 60 ° C for 8 hours to dissolve 1-ethyl-3-methylimidazolium acetate. Cellulose and chitin form a polysaccharide solution with a total solid content of 5%.

Comparative example 4

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 9:1 by weight. Next, 1-Butyl-3-methylimidazolium chloride (BMIMCl) as an ionic liquid was mixed with cellulose and chitin at 100 ° C for 8 hours to make 1 The methyl-3-butylimidazolium chloride salt dissolves cellulose and chitin to form a polysaccharide solution having a total solid content of 5%.

Comparative Example 5

First, cellulose and chitin are provided as a polysaccharide material in which the ratio of cellulose to chitin is 9:1 by weight. Next, at 100 ° C, N-methyllyllin N-oxide (N-metlylmorpholinoxid, as an ionic liquid, NMMO) was mixed with cellulose and chitin for 8 hours to dissolve the cellulose and chitin with N-methylcodein N-oxide to form a polysaccharide solution having a total solid content of 5%.

Viscosity measurement

Next, the mucus composition of Example 1 and the polysaccharide solutions of Comparative Example 2 to Comparative Example 5 were subjected to viscosity measurement, and the respective measurement results are shown in Table 2. The instruments used and the measurement parameters are as follows: Instrument: Viscometer (Model: DV-II+Pro, manufactured by Brookfield). Torque value: 90%.

Referring to Table 2, it can be seen from the experimental parameters of Example 1 and Comparative Example 2 to Comparative Example 5 that 1-methyl-3-butylimidazolium chloride salt (Comparative Example 4) and N-methylcodelin N-oxide are used. (Comparative Example 5) A higher temperature (100 ° C) was required as a solvent to dissolve cellulose and chitin (9:1 by weight ratio), and 1-Ethyl-3-methylimidazole was contained in the solvent. In Example 1, Comparative Example 2 and Comparative Example 3 of acetate, the same amount of cellulose and chitin were dissolved at a lower temperature (60 ° C). Further, the polysaccharide solution obtained by using 1-methyl-3-butylimidazolium chloride salt (Comparative Example 4) and N-methylcodein N-oxide (Comparative Example 5) as a solvent has a high viscosity in a solvent. The mucus composition of Example 1 containing 1-ethyl-3-methylimidazolium acetate and the polysaccharide solutions of Comparative Example 2 and Comparative Example 3 were all low in viscosity.

Further, from the results of the viscosity measurement of the mucus composition of Example 1 and the polysaccharide solution of Comparative Example 2 to Comparative Example 3, it was found that the addition of a small amount of dimethyl hydrazine as a solvent can lower the viscosity and further increase the processability of the mucus composition. And reduce the amount of 1-ethyl-3-methylimidazolium acetate used.

Further, from the results of the viscosity measurement of the mucus composition of Example 1 and the polysaccharide solution of Comparative Example 2, the viscosity of the mucus composition of Example 1 of the present invention was lower than that of the polysaccharide solution of Comparative Example 2. The cause of this phenomenon is presumably because dimethyl hydrazine is used as a cosolvent in Comparative Example 2, and thus dimethyl hydrazine is added together with 1-ethyl-3-methylimidazolium acetate. Cellulose and chitin are mixed. However, because dimethyl hydrazine cannot dissolve cellulose and chitin, it affects the force of 1-ethyl-3-methylimidazolium acetate to destroy the intermolecular hydrogen bond between cellulose and chitin. The solubility of ethyl-3-methylimidazolium acetate for cellulose and chitin is reduced. On the other hand, in Example 1, dimethyl hydrazine was added as a diluent after 1-ethyl-3-methylimidazolium acetate was sufficiently dissolved as a solvent, and thus a viscosity was lowered. Mucus composition. In addition, for the general coating process, the mucus composition having a viscosity of about 50,000 cPs is easier to apply and has better uniformity than the mucus composition having a viscosity of about 70,000 cPs, so the mucus composition of the present invention is preferable. Processability.

In summary, the mucus composition proposed in the above embodiment and the preparation method thereof can effectively reduce the viscosity of the mucus composition by further dissolving the polysaccharide material by using the ionic liquid, and then increasing the viscosity of the mucus composition. Processability. In addition, in the mucus composition proposed in the above embodiments and the preparation method thereof, The sub-liquid together with the diluent acts as a solvent, so that the amount of the ionic liquid used is reduced, thereby reducing the process cost.

Although the present invention has been disclosed in the above embodiments, it is not intended to limit the present invention, and any one of ordinary skill in the art can make some changes and refinements without departing from the spirit and scope of the present invention. The scope of the invention is defined by the scope of the appended claims.

S10~S14‧‧‧Steps

Claims (17)

A method for preparing a mucus composition, comprising: providing a polysaccharide material, wherein the polysaccharide material comprises a cellulose and a chitin; mixing the polysaccharide material with an ionic liquid to form a polysaccharide solution And adding a diluent to the polysaccharide solution to form the mucus composition. The method for preparing a mucus composition according to claim 1, wherein the ratio of the cellulose to the chitin is from 9:1 to 1:9 by weight. The method for preparing a mucus composition according to claim 1, wherein the ionic liquid is composed of a cation and an anion, and the cation comprises the structure represented by Formula 1: Wherein R ₁ to R ₅ are H or a hydrocarbon group having 1 to 8 carbon atoms; and the anion is one selected from the group consisting of Cl ^- , Br ^- , I ^- , CH ₃ COO ^- and HCOO ^- . The method for producing a mucus composition according to claim 1, wherein the ionic liquid comprises 1-ethyl-3-methylimidazolium acetate. The method for preparing a mucus composition according to claim 1, wherein the polysaccharide solution has a total solid content of from 1% to 25%. The method for preparing a mucus composition according to claim 1, wherein the ratio of the ionic liquid to the diluent is from 9:1 to 1:1 by weight. The method for preparing a mucus composition according to claim 1, wherein the diluent comprises dimethyl hydrazine, dimethylformamide or N-methylpyrrolidone. A mucus composition comprising: a polysaccharide material comprising a cellulose and a chitin, wherein the ratio of the cellulose to the chitin is 9:1 to 1:9 by weight, and the mucus composition is The polysaccharide material is contained in an amount of 1 wt% to 25 wt%; and an ionic liquid and a diluent, the polysaccharide material is dissolved in the ionic liquid, and the total amount of the mucus composition is The total content of the ionic liquid and the diluent is 75 wt% to 99 wt%, wherein the ratio of the ionic liquid to the diluent is 9:1 to 1:1 by weight, wherein the mucus The composition has a viscosity of from 1000 cPs to 200,000 cPs. The mucus composition according to claim 8, wherein the ratio of the cellulose to the chitin is from 9:1 to 1:1 by weight. The mucus composition according to claim 8, wherein the polysaccharide material is contained in an amount of from 1 wt% to 20 wt% based on the total weight of the mucus composition. The mucus composition according to claim 8, wherein the ionic liquid is composed of a cation and an anion, and the cation comprises the structure represented by Formula 1: Wherein R ₁ to R ₅ are H or a hydrocarbon group having 1 to 8 carbon atoms; and the anion is one selected from the group consisting of Cl ^- , Br ^- , I ^- , CH ₃ COO ^- and HCOO ^- . The mucus composition of claim 8, wherein the ionic liquid comprises 1-ethyl-3-methylimidazolium acetate (EMIMOAc). The mucus composition according to claim 8, wherein the ionic liquid and the diluent are added in a total amount of from 80% by weight to 99% by weight based on the total weight of the slime composition. The mucus composition according to claim 8, wherein the ratio of the ionic liquid to the diluent is from 5:1 to 1:1 by weight. The mucus composition of claim 8, wherein the diluent comprises dimethyl hydrazine, dimethylformamide or N-methylpyrrolidone. A polysaccharide composite material comprising: a cellulose and a chitin, wherein the ratio of the cellulose to the chitin is from 9:1 to 1:9 by weight. The polysaccharide composite according to claim 16, wherein the ratio of the cellulose to the chitin is from 9:1 to 1:1 by weight.