CN115948862B - Collagen cellulose fiber cloth and production method thereof - Google Patents
Collagen cellulose fiber cloth and production method thereof Download PDFInfo
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Abstract
The invention discloses a collagen cellulose fiber cloth and a production method thereof, belonging to the technical field of functional composite material preparation, and comprising the following steps: (1) The collagen is pretreated and then is blended with viscose to be matured, and then is spun to prepare collagen fiber; (2) Reacting the collagen fiber with itaconic anhydride to introduce unsaturated groups; introducing surface amino into the cotton fiber through an aminosilane coupling agent; (3) Mixing and carding the two materials to obtain a fiber net, and preparing the collagen cellulose fiber cloth through a non-woven fabric forming process; according to the invention, the non-woven fabric is prepared by compounding modification and compounding the cotton fiber with the reinforced fiber and the collagen fiber, and the enzymolysis resistance and mechanical property of the non-woven fabric are improved by modifying the collagen.
Description
Technical Field
The invention relates to the technical field of functional composite material preparation, in particular to a collagen cellulose fiber cloth and a production method thereof.
Background
Collagen is one of the most ubiquitous biological polymers in nature, and is a white, opaque, unbranched fibrous protein. It can supplement nutrients required by each layer of skin, enhance collagen activity in skin, and has effects in moistening skin, delaying aging, caring skin, removing wrinkles, and caring hair. Collagen is also very suitable as a tissue engineering material, because the collagen of the cow skin after digestion by pepsin does not undergo rejection reaction under the skin of the rat, and compared with the collagen, which is subjected to enzymolysis, is also deduced to have biocompatibility. There are various types of collagen known at present, among which collagen type extracted from animal skin, bone, cornea, tendon is the most clear and widely used one currently recognized. Collagen is a triple helix structure consisting of three polypeptide chains, with the amino acids on the polypeptide chains being arranged in the order glycine, proline and proline. The molecular weight is about 300kDa, the length is 300nm, and the diameter is 1.5nm. Collagen has good skin adhesion capability, biocompatibility and biodegradability, and has a promoting effect on tissue recovery, so that the collagen is widely applied to various aspects such as cosmetology, medicine, wound repair, biological tissue engineering scaffold and the like. Along with the development of functional fiber technology, the concept of collagen fiber is proposed, more and more collagen fibers and products thereof are sequentially developed, such as collagen cellulose fiber cloth and the like, collagen is compounded on a cellulose material mainly through physical adsorption preparation in the prior art, the combination between the collagen and cellulose molecules is unstable, the composite material is also unstable in performance, the pure collagen has poor mechanical property, poor degradation rate and enzyme degradation resistance or is easy to be corroded by solution, and is often required to be crosslinked by a dialdehyde crosslinking agent, but the dialdehyde crosslinking agent has toxicity problem, and the crosslinked collagen has poor processability, low flexibility, low tensile strength and easy breaking, and loses the self-functionality of the collagen.
Disclosure of Invention
In view of the above, the present invention provides a collagen cellulose fiber fabric and a method for producing the same.
The aim of the invention is realized by adopting the following technical scheme:
the production method of the collagen cellulose fiber cloth comprises the following steps:
s1, collagen fiber preparation
Dissolving collagen powder in phosphate buffer solution to prepare collagen aqueous solution with the mass fraction of 1-10% and the pH value of 7-8, heating the collagen aqueous solution to 50-65 ℃ and preserving heat for 0.5-1h to obtain collagen pretreatment solution, adding the collagen pretreatment solution into viscose according to the proportion of collagen accounting for 10-20% of the mass ratio of alpha-fiber in the viscose after cooling to room temperature, and spinning to prepare collagen nanofiber after fully mixing and continuing stirring for 4-8 h;
s2, fiber modification
Soaking the collagen nanofiber in hot dilute sodium hydroxide solution, taking out, washing with deionized water, and drying for later use; weighing itaconic anhydride and dissolving the itaconic anhydride in water or an alcohol solvent to obtain an anhydride solution, immersing the dried collagen nanofiber in the anhydride solution at normal temperature, simultaneously dropwise adding a sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 0.5-10h, separating the fiber after the reaction is completed, washing with deionized water, and drying to obtain the modified collagen nanofiber; soaking cotton fibers in hot dilute sodium hydroxide solution, rinsing with deionized water, soaking in an ethanol solution of APTMS with the mass concentration of 3-7%, washing with absolute ethanol after soaking, and drying to obtain modified cotton fibers;
s3, carding and forming
And mixing and carding the modified collagen nanofibers and the modified cotton fibers to obtain a fiber net, and preparing the collagen cellulose fiber cloth through a non-woven fabric forming process.
In some preferred embodiments, the collagen powder is type i collagen, including rat tail collagen, fish-derived collagen, bovine collagen, or porcine collagen.
In some preferred embodiments, the mass ratio of itaconic anhydride to collagen nanofibers is (0.1-6): 1.
in some preferred embodiments, the mixing mass ratio of the modified collagen nanofibers to the modified cotton fibers is (3-4): (6-7).
In some preferred embodiments, the nonwoven forming process comprises one of hydroentanglement, needle punching, hot air, hot rolling, spun bonding.
In some preferred embodiments, the web further comprises an alkynyl modified fiber, and the method of making the same comprises the steps of:
soaking the collagen nanofiber in hot dilute sodium hydroxide solution, taking out, washing with deionized water, and drying for later use; 1,6 hexanediol dipropyl acid ester is weighed and dissolved in tetrahydrofuran to prepare a solution with the concentration of 40-80mg/mL, the dried collagen nanofiber is immersed, and after standing for 2-8 hours, the collagen nanofiber is washed by tetrahydrofuran, absolute ethyl alcohol and deionized water in sequence, and the alkynyl modified fiber is prepared by drying at low temperature under flowing nitrogen.
In some preferred embodiments, the web further comprises norbornene-modified fibers, and the method of making the web comprises the steps of:
soaking the collagen nanofiber in hot dilute sodium hydroxide solution, taking out, washing with deionized water, and drying for later use; weighing norbornene dianhydride and dissolving in an alcohol solvent to obtain a norbornene dianhydride solution, immersing the dried collagen nanofiber into the norbornene dianhydride solution at normal temperature, simultaneously dropwise adding a sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 0.5-10h, separating the fiber after the reaction is completed, washing with the alcohol solvent and deionized water in sequence, and drying to obtain the norbornene modified fiber.
In some preferred embodiments, the mass ratio of the alkynyl modified fiber to the norbornene modified fiber is 1: (1-3).
Another object of the present invention is to provide a collagen cellulose fiber fabric, which is prepared by the aforementioned production method.
The beneficial effects of the invention are as follows:
according to the invention, cotton fibers are used as doped reinforced fibers to be prepared into non-woven fabrics, and the anti-enzymolysis performance and mechanical properties of the non-woven fabrics are improved through collagen fiber modification; furthermore, the invention also introduces alkynyl on the collagen fiber by taking dipropionate as a raw material, and the surface-activated alkynyl can directly react with amino on the modified cotton fiber in an alkyne-amine click way, so that high-efficiency self-crosslinking is realized, the enzymolysis resistance and mechanical property of the modified cotton fiber are further improved, and furthermore, the invention also utilizes the aminolysis of free amino and anhydride on the surface of the collagen fiber to introduce a norbornene structure with high polymerization activity, can quickly realize crosslinking copolymerization under the action of a photoinitiator, and further improves the enzymolysis resistance and mechanical property of the cloth.
Detailed Description
The invention will be further described with reference to the following examples.
Example 1
The production method of the collagen cellulose fiber cloth comprises the following steps:
s1, collagen fiber preparation
Dissolving bovine collagen powder in phosphate buffer solution to prepare collagen aqueous solution with the mass fraction of 8% and the pH value of 7-8, heating the collagen aqueous solution to 60 ℃ and preserving heat for 0.5h to obtain collagen pretreatment solution, adding the collagen pretreatment solution into viscose according to the proportion of 18% of collagen in the mass ratio of alpha-fiber in the viscose after cooling to room temperature, and spinning to prepare collagen nanofibers after fully mixing and continuing stirring for 4 h;
s2, fiber modification
Soaking the collagen nanofiber in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, taking out, washing with deionized water, and drying for later use; weighing itaconic anhydride and dissolving the itaconic anhydride in deionized water to obtain an anhydride solution, immersing the dried collagen nanofiber in the anhydride solution at normal temperature, simultaneously dropwise adding sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 2 hours, separating the fiber after the reaction is completed, washing with deionized water, and drying to obtain the modified collagen nanofiber; soaking cotton fibers in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, rinsing with deionized water, immersing in an ethanol solution of APTMS with the mass concentration of 5%, washing with absolute ethanol after the soaking is finished, and drying to obtain modified cotton fibers;
wherein, the mass ratio of the itaconic anhydride to the collagen nanofiber is 1:1, a step of;
s3, carding and forming
Mixing and carding the modified collagen nanofiber and the modified cotton fiber, wherein the mixing mass ratio of the modified collagen nanofiber to the modified cotton fiber is 3: and 7, obtaining a fiber web, and preparing the collagen cellulose fiber cloth through a water jet process.
Example 2
The production method of the collagen cellulose fiber cloth comprises the following steps:
s1, collagen fiber preparation
Dissolving bovine collagen powder in phosphate buffer solution to prepare collagen aqueous solution with the mass fraction of 8% and the pH value of 7-8, heating the collagen aqueous solution to 60 ℃ and preserving heat for 0.5h to obtain collagen pretreatment solution, adding the collagen pretreatment solution into viscose according to the proportion of 18% of collagen in the mass ratio of alpha-fiber in the viscose after cooling to room temperature, and spinning to prepare collagen nanofibers after fully mixing and continuing stirring for 4 h;
s2, fiber modification
Soaking the collagen nanofiber in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, taking out, washing with deionized water, and drying for later use; weighing itaconic anhydride and dissolving the itaconic anhydride in deionized water to obtain an anhydride solution, immersing the dried collagen nanofiber in the anhydride solution at normal temperature, simultaneously dropwise adding sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 2 hours, separating the fiber after the reaction is completed, washing with deionized water, and drying to obtain the modified collagen nanofiber; soaking cotton fibers in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, rinsing with deionized water, immersing in an ethanol solution of APTMS with the mass concentration of 5%, washing with absolute ethanol after the soaking is finished, and drying to obtain modified cotton fibers;
wherein, the mass ratio of the itaconic anhydride to the collagen nanofiber is 1:1, a step of;
s3, preparation of alkynyl modified fiber
Soaking the collagen nanofiber in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, taking out, washing with deionized water, and drying for later use; weighing 1, 6-hexanediol dipropyl acid ester, dissolving in tetrahydrofuran to prepare a solution with the concentration of 50mg/mL, immersing the dried collagen nanofiber, standing for 3 hours, washing with tetrahydrofuran, absolute ethyl alcohol and deionized water in sequence, and drying at a low temperature under flowing nitrogen to prepare the alkynyl modified fiber;
s4, carding and forming
Mixing and carding the modified collagen nanofiber, the modified cotton fiber and the alkynyl modified fiber, wherein the mixing mass ratio of the modified collagen nanofiber to the modified cotton fiber is 3:7:1, obtaining a fiber net, and preparing the collagen cellulose fiber cloth through a water jet process.
Example 3
The production method of the collagen cellulose fiber cloth comprises the following steps:
s1, collagen fiber preparation
Dissolving bovine collagen powder in phosphate buffer solution to prepare collagen aqueous solution with the mass fraction of 8% and the pH value of 7-8, heating the collagen aqueous solution to 60 ℃ and preserving heat for 0.5h to obtain collagen pretreatment solution, adding the collagen pretreatment solution into viscose according to the proportion of 18% of collagen in the mass ratio of alpha-fiber in the viscose after cooling to room temperature, and spinning to prepare collagen nanofibers after fully mixing and continuing stirring for 4 h;
s2, fiber modification
Soaking the collagen nanofiber in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, taking out, washing with deionized water, and drying for later use; weighing itaconic anhydride and dissolving the itaconic anhydride in deionized water to obtain an anhydride solution, immersing the dried collagen nanofiber in the anhydride solution at normal temperature, simultaneously dropwise adding sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 2 hours, separating the fiber after the reaction is completed, washing with deionized water, and drying to obtain the modified collagen nanofiber; soaking cotton fibers in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, rinsing with deionized water, immersing in an ethanol solution of APTMS with the mass concentration of 5%, washing with absolute ethanol after the soaking is finished, and drying to obtain modified cotton fibers;
wherein, the mass ratio of the itaconic anhydride to the collagen nanofiber is 1:1, a step of;
s3, preparation of alkynyl modified fiber
Soaking the collagen nanofiber in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, taking out, washing with deionized water, and drying for later use; weighing 1, 6-hexanediol dipropyl acid ester, dissolving in tetrahydrofuran to prepare a solution with the concentration of 50mg/mL, immersing the dried collagen nanofiber, standing for 3 hours, washing with tetrahydrofuran, absolute ethyl alcohol and deionized water in sequence, and drying at a low temperature under flowing nitrogen to prepare the alkynyl modified fiber;
s4, preparation of norbornene modified fiber
Soaking the collagen nanofiber in a dilute sodium hydroxide solution (0.01 mol/L) at 80 ℃, taking out, washing with deionized water, and drying for later use; weighing norbornene dianhydride and dissolving in an ethanol solvent to obtain a norbornene dianhydride solution, immersing the dried collagen nanofiber into the norbornene dianhydride solution at normal temperature, simultaneously dropwise adding a sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 2 hours, separating the fiber after the reaction is completed, washing with absolute ethyl alcohol and deionized water in sequence, and drying to obtain the norbornene modified fiber;
wherein the mass ratio of the norbornene dianhydride to the collagen nanofiber is 1.2:1, a step of;
s5, carding and forming
Mixing and carding the modified collagen nanofiber, the modified cotton fiber and the alkynyl modified fiber, wherein the mixing mass ratio of the modified collagen nanofiber to the modified cotton fiber is 3:7:1:1, obtaining a fiber net, preparing a non-woven fabric through a water jet process, soaking in a photoinitiator solution, and then performing ultraviolet radiation treatment to obtain the collagen cellulose fiber cloth.
Example 4
The production method of the collagen cellulose fiber cloth comprises the following steps:
s1, collagen fiber preparation
Dissolving bovine collagen powder in phosphate buffer solution to prepare collagen aqueous solution with the mass fraction of 8% and the pH value of 7-8, heating the collagen aqueous solution to 60 ℃ and preserving heat for 0.5h to obtain collagen pretreatment solution, adding the collagen pretreatment solution into viscose according to the proportion of 18% of collagen in the mass ratio of alpha-fiber in the viscose after cooling to room temperature, and spinning to prepare collagen nanofibers after fully mixing and continuing stirring for 4 h;
s2, carding and forming
Mixing and carding the collagen nanofibers and cotton fibers, wherein the mixing mass ratio of the collagen nanofibers to the cotton fibers is 3: and 7, obtaining a fiber web, and preparing the collagen cellulose fiber cloth through a water jet process.
Experimental example
1. Erosion resistance
The mass loss of the collagen cellulose fiber cloths prepared in examples 1 to 4 in a liquid environment was measured by a water immersion method, and the measurement results were as follows:
| erosion resistance | Example 1 | Example 2 | Example 3 | Example 4 |
| Mass loss/% | 0.8 | 0.5 | 0.1 | 1.1 |
2. Mechanical properties
The mechanical properties of the collagen cellulose fiber cloths prepared in examples 1 to 4 were measured, and the measurement results were as follows:
3. water resistance
The percentage of collagen loss of the collagen cellulose fiber cloths prepared in examples 1 to 4 was measured respectively at 0 to 50 times of water washing, and the measurement results were as follows:
| percent loss (%) | Example 1 | Example 2 | Example 3 | Example 4 |
| Washing with water for 0 times | 100 | 100 | 100 | 100 |
| Washing with water for 20 times | 3.7 | 3.2 | 2.4 | 14.2 |
| Washing with water for 50 times | 10.3 | 8.9 | 7.7 | 47.1 |
Resistance to enzymolysis
Regulating osmotic pressure to 250-300 mOsm by using physiological buffer saline, and adding collagenase to obtain an enzymolysis buffer solution; washing the collagen cellulose fiber cloth with clear water for several times, soaking the collagen cellulose fiber cloth in an enzymolysis buffer solution, and culturing at 30 ℃ for 24 hours, wherein the buffer solution without collagenase is used as a blank control group which is spontaneously dissolved; taking each group of reaction supernatant, measuring the content of hydroxyproline in the supernatant, subtracting the content of hydroxyproline in the collagenase-containing solution from the content of hydroxyproline in the non-collagenase-containing solution to obtain the content of hydroxyproline generated by enzymatic hydrolysis, and carrying out enzymolysis by taking the content of hydroxyproline generated by the unmodified composite nanofiber membrane as 100%, wherein the enzymolysis percentage of the modified composite nanofiber membrane is measured, and the measurement result is as follows:
| enzymolysis resistance | Example 1 | Example 2 | Example 3 | Example 4 |
| Percentage of enzymolysis/% | 10.21 | 8.14 | 6.89 | 100 |
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The production method of the collagen cellulose fiber cloth is characterized by comprising the following steps of:
s1, collagen fiber preparation
Dissolving collagen powder in phosphate buffer solution to prepare collagen aqueous solution with the mass fraction of 1-10% and the pH value of 7-8, heating the collagen aqueous solution to 50-65 ℃ and preserving heat for 0.5-1h to obtain collagen pretreatment solution, adding the collagen pretreatment solution into viscose according to the proportion of collagen accounting for 10-20% of the mass ratio of alpha-fiber in the viscose after cooling to room temperature, and spinning to prepare collagen nanofiber after fully mixing and continuing stirring for 4-8 h;
s2, fiber modification
Soaking the collagen nanofiber in hot dilute sodium hydroxide solution, taking out, washing with deionized water, and drying for later use; weighing itaconic anhydride and dissolving the itaconic anhydride in water or an alcohol solvent to obtain an anhydride solution, immersing the dried collagen nanofiber in the anhydride solution at normal temperature, simultaneously dropwise adding a sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 0.5-10h, separating the fiber after the reaction is completed, washing with deionized water, and drying to obtain the modified collagen nanofiber; soaking cotton fibers in hot dilute sodium hydroxide solution, rinsing with deionized water, soaking in an ethanol solution of APTMS with the mass concentration of 3-7%, washing with absolute ethanol after soaking, and drying to obtain modified cotton fibers;
s3, carding and forming
Mixing and carding the modified collagen nanofibers and the modified cotton fibers to obtain a fiber net, and preparing the collagen cellulose fiber cloth through a non-woven fabric forming process;
the fiber web also comprises alkynyl modified fibers, and the preparation method comprises the following steps:
soaking the collagen nanofiber in hot dilute sodium hydroxide solution, taking out, washing with deionized water, and drying for later use; weighing 1, 6-hexanediol dipropyl acid ester, dissolving in tetrahydrofuran to prepare a solution with the concentration of 40-80mg/mL, immersing the dried collagen nanofiber, standing for 2-8h, washing with tetrahydrofuran, absolute ethyl alcohol and deionized water in sequence, and drying at low temperature under flowing nitrogen to prepare the alkynyl modified fiber;
the fiber web also comprises norbornene modified fibers, and the preparation method comprises the following steps:
soaking the collagen nanofiber in hot dilute sodium hydroxide solution, taking out, washing with deionized water, and drying for later use; weighing norbornene dianhydride and dissolving in an alcohol solvent to obtain a norbornene dianhydride solution, immersing the dried collagen nanofiber into the norbornene dianhydride solution at normal temperature, simultaneously dropwise adding a sodium hydroxide solution to maintain the pH of the solution at 7-10, immersing for 0.5-10h, separating the fiber after the reaction is completed, washing with the alcohol solvent and deionized water in sequence, and drying to obtain the norbornene modified fiber.
2. The method for producing a collagen cellulose fiber fabric according to claim 1, wherein the collagen powder is type i collagen, and the type i collagen comprises rat tail collagen, fish-derived collagen, bovine collagen or porcine collagen.
3. The method for producing a collagen cellulose fiber fabric according to claim 1, wherein the mass ratio of itaconic anhydride to collagen nanofibers is (0.1-6): 1.
4. the method for producing a collagen cellulose fiber fabric according to claim 1, wherein the mixing mass ratio of the modified collagen nanofibers to the modified cotton fibers is (3-4): (6-7).
5. The method according to claim 1, wherein the non-woven fabric forming process comprises one of hydroentangling, needling, hot air and hot rolling.
6. The method for producing a collagen cellulose fiber fabric according to claim 1, wherein the mass ratio of the alkynyl modified fiber to the norbornene modified fiber is 1: (1-3).
7. Collagen cellulose fiber cloth prepared by the production method according to any one of claims 1 to 6.
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| CN102286803A (en) * | 2011-06-23 | 2011-12-21 | 阜宁澳洋科技有限责任公司 | Collagen/cellulose composite fiber and preparation method thereof |
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