CN112011222A - Ink containing hyaluronic acid and preparation method thereof - Google Patents

Abstract

The invention provides ink containing hyaluronic acid, which comprises the following components in percentage by mass: 5 to 16 percent of carbon black, 1 to 5 percent of hyaluronic acid, 5 to 13 percent of adhesive and 0.2 to 1 percent of preservative. Compared with the prior art, the ink containing hyaluronic acid has simple components, does not contain chemically synthesized preservatives such as phenol and the like, and is friendly to human body and environment; the hyaluronic acid with high and low molecular weights is added into the ink, so that the wettability of the ink during storage and use can be kept, the condensation of the ink is reduced, the writing is facilitated, meanwhile, the hyaluronic acid with high and low molecular weights can form a special net structure, and carbon black is uniformly dispersed in the net structure, so that the color of the ink is more uniform, the precipitation of the carbon black is effectively reduced, and the stability of a system is improved; the hyaluronic acid with high and low molecular weights is compounded with the adhesive, so that the buoyancy of the adhesive is improved, ink is applied to paper without being annihilated, and the writing effect is improved.

Description

Ink containing hyaluronic acid and preparation method thereof

Technical Field

The invention belongs to the field of ink, and particularly relates to ink containing hyaluronic acid and a preparation method thereof.

Background

The ink has a long history in China, is a traditional product for people to write, and is generally used for writing and drawing on rice paper, white newspaper or common paper.

The main raw materials of the ink are carbon smoke, sizing materials, additives, solution and the like, and the ink is generally prepared by mechanical processing. The rubber material is mainly plant rubber or various synthetic rubber such as acrylic rubber, polyol resin and the like besides animal rubber, in order to ensure the adhesiveness of the ink, more rubber material is generally added in the ink making process, for example, the novel ink and the making method disclosed by the patent CN102492332A comprise 10-15% of coloring agent and 12-20% of rubber material, however, the addition amount of the rubber material is too much, the ink is easy to dry and coagulate, and the ink is easy to adhere to a writing brush after being dried, so that the writing brush is difficult to clean, the service life of the writing brush is shortened, and calligraphy and paintings written by the ink with too much rubber material are easy to harden and decolor after being dried. Moreover, the ink with the common rubber material only endows the ink with certain adhesiveness, the problems of uneven dispersion of carbon smoke in an ink system and uneven color tone of the ink cannot be well solved, and the ink has poor stability, is not durably stored and can generate the phenomenon of carbon powder sinking in the storage process.

On the other hand, the sizing material is easy to decay, bad smell is easy to emit when the sizing material is added into the ink, and in order to avoid the decay problem in the storage of the ink and the painting and calligraphy, phenol is generally added into the ink to be used as a preservative, so that the long-term use of the sizing material inevitably causes damage to the environment and the human body. In the prior art, synthetic high molecular polymers are used for replacing animal glue, for example, in patent CN105802337B, the synthetic high molecular polymers are used as glue stock to prepare ink, so that the problem of stink caused by using animal glue and bone glue is solved, however, the synthetic glue is not favorable for long-time storage of painting and calligraphy due to the fact that the synthetic glue is chemically synthesized glue stock, chemical substances have certain damage to the environment and human bodies, and certain influence is also caused on writing effect.

Hyaluronic Acid (HA) is a natural mucopolysaccharide formed by alternating units of D-glucuronic Acid and N-acetylglucosamine in a linear chain. Hyaluronic acid shows a plurality of important physiological functions in organisms by virtue of unique molecular structures and physicochemical properties, and particularly has a special water retention effect, is a substance which is found to be the best in moisture retention in nature at present and is called ideal natural moisture retention factor (NMF). And the hyaluronic acid molecules are in a rigid spiral column shape in space, the inner side of the column generates strong water absorption due to the existence of a large number of hydroxyl groups, and on the other hand, due to the continuous directional arrangement of the hydroxyl groups, a hydrophobic region is formed on the molecular chain of the hyaluronic acid, so that the hyaluronic acid can form a three-dimensional network structure.

Disclosure of Invention

Aiming at the problems that the ink in the prior art is not friendly to the environment and human body, is not stored durably, is easy to coagulate and is difficult to clean and the like, the invention provides the ink containing the hyaluronic acid and the preparation method thereof.

Specifically, the present invention relates to the following aspects:

1. the ink containing the hyaluronic acid is characterized by comprising the following components in percentage by mass: 5 to 16 percent of carbon black, 1 to 5 percent of hyaluronic acid, 5 to 13 percent of adhesive and 0.2 to 1 percent of preservative.

2. The hyaluronic acid-containing ink according to claim 1, which comprises the following components in percentage by mass: 9 to 13 percent of carbon black, 2 to 3 percent of hyaluronic acid, 6 to 9 percent of adhesive and 0.3 to 0.5 percent of preservative.

3. The hyaluronic acid-containing ink according to claim 1 or 2, wherein the hyaluronic acid comprises a high molecular weight hyaluronic acid and a low molecular weight hyaluronic acid, and the mass ratio of the high molecular weight hyaluronic acid to the low molecular weight hyaluronic acid is 1-5: 1.

4. The hyaluronic acid-containing ink according to claim 3, wherein the high molecular weight hyaluronic acid has a molecular weight of 100-300 million Da, preferably 150-220 million Da, and the low molecular weight hyaluronic acid has a molecular weight of 10-90 million Da, preferably 50-70 million Da.

5. The hyaluronic acid-containing ink according to any of claims 1-4, wherein the carbon black has a particle size of 10-20 nm.

6. The hyaluronic acid-containing ink according to any of claims 1-5, wherein the adhesive is one or more selected from gum arabic, xanthan gum, guar gum, pectin, carageenan, locust bean gum, agar, and gellan gum.

7. The hyaluronic acid-containing ink according to any of claims 1-6, wherein the preservative is one or more selected from borneol, camphor, chitosan, and plant-derived preservatives.

8. A method of preparing an ink comprising hyaluronic acid, the method comprising the steps of:

dissolving the adhesive in water to prepare sol;

dissolving hyaluronic acid, carbon black and a preservative in water to obtain a mixed solution of hyaluronic acid and carbon black;

mixing the sol with the hyaluronic acid and carbon black mixed solution, and grinding to obtain a grinding fluid;

and filtering the grinding liquid to obtain the ink containing hyaluronic acid.

9. The method of preparing a hyaluronic acid-containing ink according to claim 8, wherein the forming of the hyaluronic acid and carbon black mixed solution comprises the steps of:

dissolving hyaluronic acid in water to obtain a hyaluronic acid solution;

dissolving carbon black and a preservative in water to obtain a carbon black solution;

and dropwise adding the carbon black solution into the hyaluronic acid solution under stirring to obtain a mixed solution of hyaluronic acid and carbon black.

10. The method for preparing an ink containing hyaluronic acid according to claim 8 or 9, wherein the ink containing hyaluronic acid comprises, by mass, 5% to 16% of carbon black, 1% to 5% of hyaluronic acid, 5% to 13% of an adhesive, and 0.2% to 1% of a preservative.

11. The method according to claim 10, wherein the ink containing hyaluronic acid comprises, by mass, 9% to 13% of carbon black, 2% to 3% of hyaluronic acid, 6% to 9% of an adhesive, and 0.3% to 0.5% of a preservative.

12. The method for preparing a hyaluronic acid-containing ink according to any of claims 8 to 11, wherein the hyaluronic acid comprises a high molecular weight hyaluronic acid and a low molecular weight hyaluronic acid, and the mass ratio of the high molecular weight hyaluronic acid to the low molecular weight hyaluronic acid is 1-5: 1.

13. The method of any one of claims 8 to 12, wherein the high molecular weight hyaluronic acid has a molecular weight of from 100 to 300 million Da, preferably from 150 to 220 million Da, and the low molecular weight hyaluronic acid has a molecular weight of from 10 to 90 million Da, preferably from 50 to 70 million Da.

14. The method of preparing a hyaluronic acid-containing ink according to any of claims 8-13, wherein the carbon black has a particle size of 10-20 nm.

15. The method of preparing an ink containing hyaluronic acid according to any of claims 8 to 14, wherein the adhesive is one or more selected from gum arabic, xanthan gum, guar gum, pectin, carageenan, locust bean gum, agar, and gellan gum.

16. The method for preparing an ink containing hyaluronic acid according to any of claims 8 to 15, wherein the preservative is one or two selected from borneol, camphor, chitosan, and plant-extracted preservatives.

17. The method of preparing a hyaluronic acid-containing ink according to any of claims 8-16, wherein the preparing the sol comprises the steps of: dissolving the adhesive in water, heating to 80-90 ℃, and swelling for 1-2h to obtain the sol.

Compared with the prior art, the ink containing hyaluronic acid has the following beneficial effects:

1. the ink has simple components, does not contain chemically synthesized preservatives such as phenol and the like, and is friendly to human body and environment;

2. hyaluronic acid is added into the ink, so that the using amount of an adhesive is reduced, the problems that the ink is easy to congeal and is difficult to clean and the like are solved, and the service life of the writing brush is prolonged;

3. the hyaluronic acid with high and low molecular weights is added into the ink, so that the ink and the wettability during use can be maintained, the condensation of the ink is reduced, the writing is facilitated, meanwhile, the hyaluronic acid with high and low molecular weights can form a special net structure, carbon black can be uniformly dispersed in the net structure, the color of the ink is more uniform, and the carbon black is dispersed in the net structure, so that the precipitation of the carbon black is reduced, and the stability of a system is improved;

4. the hyaluronic acid with high and low molecular weights is compounded with the adhesive, so that the buoyancy of the Arabic gum is improved, the ink can be pasted on paper without being annihilated, meanwhile, the adhesive strength of the ink is improved, the brush pen dipped with the ink is firmer and gathered, and the writing effect is improved.

Drawings

FIG. 1 is a graph showing the positive effects of writing with an ink containing hyaluronic acid according to example 1 of the present invention;

FIG. 2 is a front effect view of morning ink writing;

FIG. 3 is a graph showing the negative effects of writing with an ink containing hyaluronic acid according to example 1 of the present invention;

FIG. 4 is a reverse effect of morning ink writing.

Detailed Description

The present invention is further illustrated by the following examples, which are intended to be purely exemplary of the invention and are not intended to be limiting.

Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. Although methods and materials similar or equivalent to those described herein can be used in experimental or practical applications, the materials and methods are described below. In case of conflict, the present specification, including definitions, will control, and the materials, methods, and examples are illustrative only and not intended to be limiting. The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.

As mentioned above, in the prior art, which is not friendly to the environment and human body, is not durable, and is liable to coagulate and difficult to clean, Hyaluronic Acid (HA), which is a natural mucopolysaccharide, is formed of alternating units of D-glucuronic Acid and N-acetylglucosamine in a straight chain. Hyaluronic acid has a special water retention effect, is the best natural moisturizing substance discovered at present in the nature, and is called ideal Natural Moisturizing Factor (NMF).

According to the ink, the hyaluronic acid is added into the ink, so that the wettability of the ink during storage and use can be kept, the condensation of the ink is reduced, the writing is facilitated, meanwhile, the hyaluronic acid can form a special net structure, carbon black can be uniformly dispersed in the net structure, the color of the ink is more uniform, the carbon black is dispersed in the net structure, the precipitation of the carbon black is reduced, and the stability of a system is improved; in addition, the hyaluronic acid and the adhesive are compounded, so that the buoyancy of the adhesive is improved, ink is coated on paper and is not annihilated, the adhesive strength of ink is improved while the using amount of the adhesive is reduced, a writing brush dipped with the ink is firmer and gathered, the writing effect is improved, and the service life of the writing brush is prolonged.

Specifically, the invention provides ink containing hyaluronic acid, which comprises the following components in percentage by mass: 5 to 16 percent of carbon black, 1 to 5 percent of hyaluronic acid, 5 to 13 percent of adhesive and 0.2 to 1 percent of preservative. The carbon black is 5% to 16%, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, preferably 9% to 13%. The hyaluronic acid is 1% to 5%, and may be, for example, 1%, 2%, 3%, 4%, 5%, and preferably 2% to 3%. The amount of the binder is 5% to 13%, and may be, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, preferably 6% to 9%. The preservative is 0.2% to 1%, and may be, for example, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.9%, 1%, and preferably 0.3% to 0.5%. The balance of the ink containing hyaluronic acid is water.

The hyaluronic acid may be of any molecular weight, and in a preferred embodiment, the hyaluronic acid comprises a high molecular weight hyaluronic acid and a low molecular weight hyaluronic acid, and the mass ratio of the high molecular weight hyaluronic acid to the low molecular weight hyaluronic acid is 1-5:1 may be, for example, 1:1, 2:1, 3:1, 4:1 or 5: 1. The molecular weight of the high molecular weight hyaluronic acid is 100-300 million Da, for example, 100-ten thousand Da, 120-ten thousand Da, 150-ten thousand Da, 180-ten thousand Da, 200-ten thousand Da, 220-ten thousand Da, 250-ten thousand Da, 280-ten thousand Da, 300-ten thousand Da, preferably 150-220-ten thousand Da. The low molecular weight hyaluronic acid has a molecular weight of 10 to 90 million Da, for example, 10 to 20, 30, 40, 50, 60, 70, 80, 90, preferably 50 to 70 million Da.

Carbon black, also known as carbon black, is an amorphous carbon. Light, loose and extremely fine black powder with very large surface area ranging from 10 to 3000m²The carbon-containing substance is a product obtained by incomplete combustion or thermal decomposition of a carbon-containing substance (coal, natural gas, heavy oil, fuel oil, etc.) under the condition of insufficient air. Can be used as black dye for manufacturing Chinese ink, printing ink, etc. In a preferred embodiment, the carbon black used in the present invention has a particle size of 10 to 20nm, where the particle size refers to the geometric mean diameter of the carbon black particles.

The ink containing the hyaluronic acid is mainly used for improving the adhesiveness of the ink, so that the ink can be used for writing paper, and meanwhile, a writing brush dipped with the ink is firmer and gathered, and the writing effect is improved. The adhesive is one or more than two of acacia gum, xanthan gum, guar gum, pectin, carrageenin, locust bean gum, agar and gellan gum, and can be one or two or three of the acacia gum, the xanthan gum, the guar gum, the pectin, the carrageenin, the locust bean gum, the agar and the gellan gum.

Among them, gum arabic is also called gum arabic, which is derived from the stem exudate of acacia belonging to the family leguminosae, and is therefore also called acacia. Arabic gum contains high molecular polysaccharides and its calcium, magnesium and potassium salts. Mainly comprises arabinose, galactose, glucuronic acid and the like. The acacia gum with good quality is amber, has large and round particles and is mainly produced in Africa. At present, the acacia gum is also in powder form obtained by a refining process, and the use is more convenient.

The antiseptic is one or two selected from Borneolum, Camphora, chitosan, and plant extract antiseptic. The plant extract antiseptic may be Scutellariae radix extract, Aloe extract, green tea extract, etc.

The invention also provides a preparation method of the ink containing hyaluronic acid, which comprises the following steps: dissolving the adhesive in water to prepare sol; dissolving hyaluronic acid, carbon black and a preservative in water to obtain a mixed solution of hyaluronic acid and carbon black; mixing the sol with the hyaluronic acid and carbon black mixed solution, and grinding to obtain a grinding fluid; and filtering the grinding liquid to obtain the ink containing hyaluronic acid.

In a specific embodiment, the preparation of the sol comprises the steps of: dissolving the adhesive in water, heating to 80-90 ℃, and swelling for 1-2h to obtain the sol.

The hyaluronic acid, the carbon black and the preservative are dissolved in water and uniformly mixed to form the hyaluronic acid and carbon black mixed solution, and the hyaluronic acid, the carbon black and the preservative can be added and uniformly mixed in any mode. In a specific embodiment, the forming of the hyaluronic acid and carbon black mixed solution comprises the steps of: dissolving hyaluronic acid in water to obtain a hyaluronic acid solution; dissolving carbon black and a preservative in water to obtain a carbon black solution; and dropwise adding the carbon black solution into the hyaluronic acid solution under stirring to obtain a mixed solution of hyaluronic acid and carbon black. The preparation step of dropwise adding the carbon black solution into the hyaluronic acid solution under stirring can make the mixing more uniform, and can make the carbon black uniformly dispersed in a network structure formed by compounding hyaluronic acid.

According to the mass percentage of the ink containing hyaluronic acid, the prepared ink containing hyaluronic acid contains 5% -16% of carbon black, 1% -5% of hyaluronic acid, 5% -13% of an adhesive and 0.2% -1% of a preservative. The carbon black is 5% to 16%, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, preferably 9% to 13%. The hyaluronic acid is 1% to 5%, and may be, for example, 1%, 2%, 3%, 4%, 5%, and preferably 2% to 3%. The amount of the binder is 5% to 13%, and may be, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, preferably 6% to 9%. The preservative is 0.2% to 1%, and may be, for example, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.9%, 1%, and preferably 0.3% to 0.5%.

The hyaluronic acid may be of any molecular weight, and in a preferred embodiment, the hyaluronic acid comprises a high molecular weight hyaluronic acid and a low molecular weight hyaluronic acid, and the mass ratio of the high molecular weight hyaluronic acid to the low molecular weight hyaluronic acid is 1-5:1, and may be, for example, 1:1, 2:1, 3:1, 4:1, 5: 1. The molecular weight of the high molecular weight hyaluronic acid is 100-300 million Da, for example, 100-ten thousand Da, 120-ten thousand Da, 150-ten thousand Da, 180-ten thousand Da, 200-ten thousand Da, 220-ten thousand Da, 250-ten thousand Da, 280-ten thousand Da, 300-ten thousand Da, preferably 150-220-ten thousand Da. The low molecular weight hyaluronic acid has a molecular weight of 10 to 90 million Da, for example, 10 to 20, 30, 40, 50, 60, 70, 80, 90, preferably 50 to 70 million Da.

The adhesive is one or more than two of acacia gum, xanthan gum, guar gum, pectin, carrageenin, locust bean gum, agar and gellan gum, and can be one or two or three of the acacia gum, the xanthan gum, the guar gum, the pectin, the carrageenin, the locust bean gum, the agar and the gellan gum. The antiseptic is one or two selected from Borneolum, Camphora, chitosan, and plant extract antiseptic.

The ink containing hyaluronic acid provided by the invention improves the stability of the ink, and particularly, when the molecular weight of high molecular weight hyaluronic acid of 150w-220wDa and the molecular weight of low molecular weight hyaluronic acid of 50w-70wDa are in a ratio of 1-5:1, the ink is compounded with Arabic gum and carbon black, the content of hyaluronic acid is 2-3%, the content of Arabic gum is 6-9%, the content of carbon black is 9-13%, the ink system is most stable, and the ink can reach the level of middle and high grade products in color, centrifugal color and diffusion; the ink does not leak after being soaked for 6 hours, is recovered after being frozen, the physical and chemical properties of the stock solution reach the standard specified index, and the stock solution has no peculiar smell after an anti-corrosion test, the ink liquid is not frozen after the test and can be normally used, and the thermal stability is not abnormal, so the ink has excellent physical and chemical properties; the ink has better effect on calligraphy than the prior ink, has the effect of preventing ink from running out when water runs on rice paper, and has the effects of preventing the ink from running out when the ink is stuck on the paper, and preventing the ink from permeating the back of the paper and diffusing.

Examples

Example 1

Dissolving 8g of Arabic gum in 50ml of water, heating to 90 ℃, and swelling for 2 hours to form sol;

adding 2.4g of high molecular weight hyaluronic acid (180 ten thousand Da) and 0.6g of low molecular weight hyaluronic acid (60 ten thousand Da) into 20ml of water, and fully stirring and dissolving uniformly to obtain a hyaluronic acid solution; dissolving 10g of carbon black and 0.5g of borneol in 30ml of water, and fully stirring and uniformly dissolving to obtain a carbon black solution, wherein the particle size of the carbon black is 10 nm; dropwise adding the carbon black solution into the hyaluronic acid solution under stirring to obtain a mixed solution of hyaluronic acid and carbon black;

mixing the sol, hyaluronic acid and carbon black mixed solution, and grinding to obtain grinding fluid; and sieving the obtained grinding liquid with a 100-mesh sieve to obtain the ink containing hyaluronic acid.

Example 2

Example 2 is different from example 1 in the molecular weight and mass of hyaluronic acid added, the mass of gum arabic, and the mass of carbon black, and other reaction conditions are the same as example 1. Specifically, as shown in Table 1, 1.5g of high molecular weight hyaluronic acid (220 ten thousand Da) and 0.5g of low molecular weight hyaluronic acid (50 ten thousand Da), 9g of gum arabic, and 13g of carbon black were added.

Example 3

Example 3 is different from example 1 in the molecular weight and mass of hyaluronic acid added, the mass of gum arabic, and the mass of carbon black, and other reaction conditions are the same as example 1. Specifically, as shown in Table 1, 2g of high molecular weight hyaluronic acid (150 ten thousand Da) and 1g of low molecular weight hyaluronic acid (70 ten thousand Da), 6g of gum arabic, and 9g of carbon black were added.

Example 4

Example 4 is different from example 1 in the molecular weight and mass of hyaluronic acid added, the mass of gum arabic, and the mass of carbon black, and other reaction conditions are the same as example 1. Specifically, as shown in Table 1, 4g of high molecular weight hyaluronic acid (100 ten thousand Da) and 1g of low molecular weight hyaluronic acid (10 ten thousand Da), 5g of gum arabic, and 5g of carbon black were added.

Example 5

Example 5 is different from example 1 in the molecular weight and mass of hyaluronic acid added, the mass of gum arabic, and the mass of carbon black, and other reaction conditions are the same as example 1. Specifically, as shown in Table 1, 0.5g of high molecular weight hyaluronic acid (300 ten thousand Da) and 0.5g of low molecular weight hyaluronic acid (90 ten thousand Da), 13g of gum arabic, and 16g of carbon black were added.

Example 6

Example 6 is different from example 1 in that the procedure for preparing a mixed solution of hyaluronic acid and carbon black is different, and other reaction conditions are the same as example 1. Specifically, the operation steps are as follows: 2.4g of high molecular weight hyaluronic acid (180 ten thousand Da), 0.6g of low molecular weight hyaluronic acid (60 ten thousand Da), 10g of carbon black and 0.5g of antiseptic borneol are dissolved in 50ml of water, and the mixture is fully stirred and uniformly mixed to obtain a mixed solution of the hyaluronic acid and the carbon black.

Comparative example 1

Comparative example 1 is different from example 1 in the molecular weight of low molecular weight hyaluronic acid added, and other reaction conditions are the same as example 1. Specifically, as shown in Table 1, the molecular weight of the low molecular weight hyaluronic acid added was 5 ten thousand Da.

Comparative example 2

Comparative example 2 is different from example 1 in that only high molecular weight hyaluronic acid is added and low molecular weight hyaluronic acid is not added, and specifically, as shown in table 1, other reaction conditions are the same as example 1.

Comparative example 3

Comparative example 3 is different from example 1 in that only low molecular weight hyaluronic acid is added and high molecular weight hyaluronic acid is not added, and specifically, as shown in table 1, other reaction conditions are the same as example 1.

Comparative example 4

Comparative example 4 differs from example 1 in that hyaluronic acid was not added and the other components were added in the same amounts as in example 1, specifically, as shown in table 1. The specific operation steps are that 6g of acacia gum as an adhesive is dissolved in 50ml of water, the water is heated to 90 ℃, and swelling is carried out for 2 hours to form sol; dissolving 9g of carbon black and 0.5g of antiseptic borneol in 50ml of water, fully stirring and uniformly dissolving to obtain a carbon black solution, wherein the particle size of the carbon black is 10 nm; mixing the sol and the carbon black solution, and grinding to obtain a grinding fluid; and sieving the obtained grinding liquid with a 100-mesh sieve to obtain the ink.

Comparative example 5

Comparative example 5 is different from example 1 in that the molecular weight of the high molecular weight hyaluronic acid added is 400 ten thousand Da, and other reaction conditions are the same as example 1, specifically, as shown in table 1.

Comparative example 6

Comparative example 6 differs from example 1 in the total mass and ratio of hyaluronic acid added, specifically, as shown in Table 1, 2.0g of high molecular weight hyaluronic acid (180 ten thousand Da) and 4.0g of low molecular weight hyaluronic acid (70 ten thousand Da) were added

TABLE 1 contents of components of different examples and comparative examples

Test example 1 stability test

Diluting the ink prepared in the examples 1-6 and the ink prepared in the comparative examples 1-6 by 1000 times (mass ratio) by using deionized water, then carrying out ultrasonic treatment, and centrifuging the diluted sample by using a centrifugal tube; the diluted samples were centrifuged at 0, 1000, 1500, 2000 rpm for 5 minutes using a bench-top high speed centrifuge (Hunan instrument Power test instruments, Inc., TG16-WS), respectively; then, absorbance values of the centrifuged samples at a wavelength of 540nm were measured using an ultraviolet-visible-near infrared spectrophotometer (Hitachi, Japan, U4150), respectively, and then specific absorbances A1/A were calculated, wherein A is the absorbance before centrifugation and A1 is the absorbance after centrifugation. The closer the specific absorbance is to 1, the more stable the system, and the specific stability results are shown in table 2.

TABLE 2

According to the invention, through reasonable compounding of hyaluronic acid and Arabic gum with different molecular weights, the ink has better stability. As can be seen from the above table, the values of examples 1-5 are above 0.90, especially when the ratio of high molecular weight hyaluronic acid of 150w-220wDa to low molecular weight hyaluronic acid of 50w-70wDa is 1-5:1, the ink is compounded with Arabic gum and carbon black, and the ink system is most stable when the content of hyaluronic acid is 2-3%, the content of Arabic gum is 6-9% and the content of carbon black is 9-13%; example 6 was slightly less stable than examples 1-5 due to its preparation by conventional methods, and had a specific absorbance of 0.88. The low molecular weight hyaluronic acid adopted in the comparative example 1 has too low molecular weight, and the high molecular weight hyaluronic acid adopted in the comparative example 5 has too high molecular weight, which is not beneficial to the stability of the ink; in comparative example 6, the content of hyaluronic acid is higher and the mass ratio of high-molecular weight hyaluronic acid to low-molecular weight hyaluronic acid is not properly selected, so that the stability of the ink is poor; comparative examples 2 and 3, which only contain hyaluronic acid with one molecular weight, have certain influence on the stability of the ink, but the stability of comparative example 2, which only contains hyaluronic acid with high molecular weight, is obviously higher than that of comparative example 3, which only contains hyaluronic acid with low molecular weight, so that the contribution of hyaluronic acid with high molecular weight is larger than that of hyaluronic acid with low molecular weight although both hyaluronic acid with high molecular weight contributes to the stability of the ink system; comparative example 4 contained no hyaluronic acid, the system stability was the worst, and carbon black precipitation after centrifugation was significant.

Test example 2 measurement of physical and chemical indexes

1. Test method

The products in the embodiment and the comparative example of the invention detect the physical and chemical indexes according to the light industry standard QB/T2860-2007 of the people's republic of China.

Detecting items: color, centrifugal color, diffusion, water resistance, cold resistance, corrosion resistance, use environment requirement and heat storage stability.

The physicochemical properties were as shown in Table 3.

TABLE 3 index of physicochemical Properties

2. Test results

The evaluation results of the physicochemical properties of each example and comparative example are shown in Table 4. Test example 1 stability test

TABLE 4 evaluation results of physicochemical Properties of examples and comparative examples

The inks prepared in the examples of the present invention all achieved intermediate quality, particularly the inks prepared in examples 1-3 achieved superior quality, particularly the ink prepared in example 1 was the best, and the ink prepared in example 6 was slightly inferior but better than the comparative examples in the method of preparation, unlike the methods of preparation in examples 1-5. The inks prepared in the comparative examples are inferior to the inks prepared in the examples in color, degree of uniform diffusion and water resistance, which shows that the addition amount of hyaluronic acid, the molecular weight and the proportion of high molecular weight hyaluronic acid and low molecular weight hyaluronic acid in hyaluronic acid have an influence on the quality of the inks, and the preparation method in example 1 can improve the quality of the inks to a certain extent for raw materials with the same composition.

Test example 3 ink writing effect test

To illustrate the ink effect of the present invention more intuitively, we chose to compare the ink made in example 1 with a conventional ink (morning ink) currently on the market.

The test method comprises the following steps: the same Chinese brush is used for dipping different ink on the same raw Xuan paper to write the effect picture of the same character.

Wherein FIG. 1 is a diagram showing the positive effects of writing with an ink containing hyaluronic acid according to example 1 of the present invention; FIG. 2 is a front effect view of morning ink writing; FIG. 3 is a graph showing the negative effects of writing with an ink containing hyaluronic acid according to example 1 of the present invention; FIG. 4 is a reverse effect of morning ink writing.

The ink has better calligraphy effect than the prior ink, has the effect of preventing ink from running on rice paper, is adhered to the paper without being destroyed, and has the effects of not penetrating the back of the paper and not diffusing.

Claims (10)

1. The ink containing the hyaluronic acid is characterized by comprising the following components in percentage by mass: 5 to 16 percent of carbon black, 1 to 5 percent of hyaluronic acid, 5 to 13 percent of adhesive and 0.2 to 1 percent of preservative.

2. The hyaluronic acid-containing ink according to claim 1, which comprises the following components in percentage by mass: 9 to 13 percent of carbon black, 2 to 3 percent of hyaluronic acid, 6 to 9 percent of adhesive and 0.3 to 0.5 percent of preservative.

3. The hyaluronic acid-containing ink according to claim 1 or 2, wherein the hyaluronic acid comprises a high molecular weight hyaluronic acid and a low molecular weight hyaluronic acid, and the mass ratio of the high molecular weight hyaluronic acid to the low molecular weight hyaluronic acid is 1-5: 1.

4. A hyaluronic acid-containing ink as claimed in claim 3, wherein the high molecular weight hyaluronic acid has a molecular weight in the range 100 to 300 million Da, preferably 150 to 220 million Da, and the low molecular weight hyaluronic acid has a molecular weight in the range 10 to 90 million Da, preferably 50 to 70 million Da.

5. The hyaluronic acid-containing ink according to any of claims 1-4, wherein the carbon black has a particle size of 10-20 nm.

6. The hyaluronic acid-containing ink according to any of claims 1-5, wherein the adhesive is one or more selected from gum arabic, xanthan gum, guar gum, pectin, carageenan, locust bean gum, agar, gellan gum.

7. The hyaluronic acid-containing ink according to any of claims 1-6, wherein the preservative is one or more selected from borneol, camphor, chitosan, plant-derived preservatives.

8. A method of preparing an ink comprising hyaluronic acid, the method comprising the steps of:

dissolving the adhesive in water to prepare sol;

dissolving hyaluronic acid, carbon black and a preservative in water to obtain a mixed solution of hyaluronic acid and carbon black;

mixing the sol with the hyaluronic acid and carbon black mixed solution, and grinding to obtain a grinding fluid;

and filtering the grinding liquid to obtain the ink containing hyaluronic acid.

9. The method of preparing a hyaluronic acid-containing ink as claimed in claim 8, wherein the forming of the hyaluronic acid and carbon black mixed solution comprises the steps of:

dissolving hyaluronic acid in water to obtain a hyaluronic acid solution;

dissolving carbon black and a preservative in water to obtain a carbon black solution;

and dropwise adding the carbon black solution into the hyaluronic acid solution under stirring to obtain a mixed solution of hyaluronic acid and carbon black.

10. The method for preparing an ink containing hyaluronic acid according to claim 8 or 9, wherein the ink containing hyaluronic acid comprises, by mass, 5% to 16% of carbon black, 1% to 5% of hyaluronic acid, 5% to 13% of an adhesive, and 0.2% to 1% of a preservative.

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