CN114438771A - Preparation method of biological hyaluronic acid flame-retardant polyester cotton based on complexation of reactive sericin and metal ions - Google Patents
Preparation method of biological hyaluronic acid flame-retardant polyester cotton based on complexation of reactive sericin and metal ions Download PDFInfo
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- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
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- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
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- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The invention discloses a preparation method of biological hyaluronic acid flame-retardant polyester cotton based on reactive sericin and metal ion complexation, which comprises the steps of firstly carrying out plasma treatment on cotton fabric, then further treating the polyester cotton fabric by using a sodium periodate solution, increasing active groups on the surface of the polyester cotton fabric, chemically bonding the sericin and the modified polyester cotton fabric, then respectively further reacting the polyester cotton fabric with a biomass acid solution, finally spraying different metal ions on the surface of the polyester cotton fabric to carry out complexation reaction with the biological hyaluronic acid, and finally preparing the biological hyaluronic acid flame-retardant polyester cotton based on reactive sericin and metal ion complexation. The biomass flame-retardant finishing agent has wide sources, is a full utilization of waste materials in the silk product process, is a flame-retardant finishing agent with lower cost and environmental protection, and finishes the flame retardant on the surface of the polyester-cotton fabric by utilizing a chemical key joint mode, thereby increasing the adhesive force of the flame retardant on the surface of the fabric, improving the durability of the flame-retardant fabric, prolonging the service life of the textile and having good practical value.
Description
Technical Field
The invention relates to the field of production of biomass flame-retardant textile materials, in particular to a method for complexing biological hyaluronic acid flame-retardant polyester cotton based on reactive sericin and metal ions.
Background
With the progress of society and the development of science and technology, the consumption and variety of polyester cotton are on a trend of increasing sharply year by year. Because the polyester cotton has the advantages of good moisture absorption and air permeability, excellent mechanical strength, low price, simple preparation process and the like, the polyester cotton occupies an important position in the modern textile industry, however, the polyester cotton has extremely high combustion risk, has high fire spreading speed and strong combustion-supporting performance in the combustion process, and is very easy to threaten the life safety of personnel. With the increasing awareness of fire safety, how to slow down the burning of polyester cotton has become one of the problems that all countries in the world pay attention to and try to solve in recent years. Currently, organic flame retardant is widely regarded by scholars at home and abroad due to its advantages of low smoke, low toxicity, no halogen, high-efficiency flame retardation. However, the raw materials of formaldehyde and intermediate bischloromethyl ether used in the preparation process of the phosphorus flame-retardant finishing agent are carcinogenic to human bodies, and the method has great danger. Meanwhile, inorganic phosphorus-based flame-retardant fibers are questioned due to the problems of large smoke generation, toxic smoke generation after combustion, environmental pollution and the like.
The combination of flame-retardant fiber preparation, fabric flame-retardant coating finishing, flame-retardant fiber and flame-retardant finishing is the main method for preparing flame-retardant textiles at present. For example, Huyuan et al [ Carbohydrate polymers.15August 2017, Pages133-139] of the university of Chinese science and technology prepares a modified cotton fabric by a layer-by-layer assembly method using positively charged polyethyleneimine and negatively charged alginate. Then, metal ions are successfully constructed on the substrate, and the degradation of the cotton fabric at high temperature is found to be inhibited. The research provides an idea for fully utilizing metal ions to crosslink the alginate so as to endow the fabric with excellent flame retardant property. Pen\25035et al (Chinese Journal of Polymer Science volume 32, pages 305-314 (2014)) at university of Zhejiang prepares a novel intumescent flame retardant coating on the surface of ramie fabric by using polyvinyl phosphonic acid (PVPA) as an acid source and Branched Polyethyleneimine (BPEI) as a foaming agent and adopting an alternative layer-by-layer self-assembly method. The surface of the ramie fabric single fiber is pyrolyzed by the PVPA/BPEI coating to form a protective carbon layer, so that the flame retardant property of the ramie is improved. The result shows that the residual quantity of the PVPA/BPEI coating ramie fabric at 600 ℃ reaches 25.8%, the total heat release quantity of the PVPA/BPEI coating is reduced by 66% and the heat release quantity is reduced by 76% compared with that of an uncoated fabric, the research improves the fire resistance of the fiber, provides a promising strategy for the design of char flame retardance, and widens the application of the fiber in functional fireproof high polymer materials by taking various high polymer phases as flame retardant elements. Although the layer-by-layer self-assembly technology is a universal, economic and effective multifunctional preparation method, the bonding force of the assembly technology is often due to the defects of weak adhesion, easy falling and the like, the durability of the flame-retardant textile is shortened, a large amount of manual operation is needed in the industrial application process, the cross contamination risk among solutions can be generated in the application process, and the weather resistance of the flame-retardant coating is influenced by repetitive physical friction, water washing, bacterial erosion and the like in the processing process. So that the application technology still has no indication of industrial production, and new flame retardant material/method research is needed to promote the development of the application technology.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of biological hyaluronic acid flame-retardant polyester cotton based on reaction type sericin and metal ion complexation, which comprises the steps of firstly carrying out plasma treatment on the surface of a fabric, removing grease, slurry and impurities on the surface of the fiber, then carrying out oxidation treatment on the surface of the polyester cotton fabric by using a sodium periodate solution, increasing active groups on the surface of the polyester cotton fabric, then carrying out Schiff base reaction to chemically bond the sericin and the modified polyester cotton fabric, then carrying out reaction with the biological hyaluronic acid, and finally spraying different metal ion solutions for complexation reaction The clothing and other fields have good popularization value.
The invention provides a preparation method of a reactive sericin and metal ion complexing biological hyaluronic acid flame-retardant fabric, which is easy to implement and simple in process and is based on a preparation method of various biomass flame-retardant materials and combines a chemical bond technology to improve the firmness of a flame-retardant finishing agent.
A preparation method of biological hyaluronic acid flame-retardant polyester cotton based on complexation of reactive sericin and metal ions comprises the following steps:
s1, firstly, putting the polyester cotton into a plasma processor to process the surface of the polyester cotton for a certain time, and removing the sizing agent and various additives on the surface of the polyester cotton;
s2, selectively oxidizing the surface of the polyester-cotton fabric by using a strong oxidant solution, chemically bonding sericin with the modified polyester-cotton fabric by using Schiff base reaction, further reacting the polyester-cotton fabric with different biological hyaluronic acids respectively, and finishing the biological hyaluronic acids on the surface of the modified polyester-cotton fabric for later use;
s3, respectively spraying different metal ion solutions on the polyester-cotton fabric manufactured in the S2 to enable the polyester-cotton fabric to be complexed with the biological hyaluronic acid, and thus, the flame-retardant coating polyester-cotton fabric with the reactive sericin and the metal ion complexed biological hyaluronic acid is manufactured.
Preferably, in the step S1, the processing time of the plasma processing is 3-20 min.
Preferably, in the step S1, the content of the polyester in the polyester-cotton fabric is 5% to 100%.
Preferably, in step S2, the strong oxidant is one or more of sodium periodate, sodium hypochlorite, and hydrogen peroxide.
Preferably, the concentration of the strong oxidant solution in the step S2 is 5g/L-20 g/L.
Preferably, in the step S2, the content of sericin is 10 to 100 g/L. The loading capacity on the surface of the polyester-cotton fabric is 20-60g/m2。
Preferably, in the step S2, the content of the aqueous biomass acid solution is 1g/L-10 g/L. The loading capacity on the surface of the polyester-cotton fabric is 1-10g/m2。
Preferably, in step S2, the biological acid is one or more of alginic acid, tannin and phytic acid.
Preferably, in step S3, the different metal ions include: fe3+、Mg2+、Cu2+、Ba2+、Co2+、Ni2+One or more of plasma metal ions, wherein the concentration of the metal ion solution is 1g/L-10g/L, and the spraying amount of the metal ion solution is 1g/m2-10g/m2。
The flame-retardant polyester cotton based on the reactive sericin and metal ion complexing biological hyaluronic acid is prepared by any one of the methods.
The core idea of the invention is to provide a preparation method of a biological hyaluronic acid flame retardant fabric by complexing biomass protein and metal ions, firstly, grease, slurry and other impurities on the surface of the fabric are subjected to preliminary treatment by plasma treatment to increase active groups on the surface of the fabric, then sodium periodate solution is used for carrying out oxidation treatment on the surface of polyester-cotton fabric, -CHO groups on the surface of the polyester-cotton fabric are increased, sericin protein and modified polyester-cotton fabric are chemically bonded by Schiff base reaction and then react with biological hyaluronic acid, finally different metal ions are sprayed for carrying out complex reaction, and the flame retardant finishing agent with different metal ions complexing is obtained after the ion exchange and complex reaction between the metal ions and the biological hyaluronic acid, the method for preparing the flame retardant finishing agent by biomass raw materials has the advantages of easy obtainment of raw materials, simple method and innovative utilization of synergistic flame retardant behavior of protein and biological hyaluronic acid, carcinogens such as formaldehyde, bischloromethyl ether and the like generated in preparation and use of the existing phosphorus flame retardant are eliminated, and meanwhile, the flame retardant finishing agent is in key joint with the surface of the polyester-cotton fabric by utilizing a chemical bond, so that the flame retardant durability and firmness of the polyester-cotton fabric are improved, and a new design method is expected to be provided for the environment-friendly, green and low-toxicity flame retardant finishing agent.
Compared with the prior art, the invention has the following beneficial effects:
based on the traditional flame-retardant finishing agent, the invention uses innovative raw materials. In particular, conventional flame retardant finishes release toxic gases and carcinogens both during use and preparation. With the enhancement of social environmental awareness, researchers have raised the attention on nontoxic and environment-friendly flame retardants, and sericin and biological hyaluronic acid used in the flame retardant can solve the problems of the release of harmful gases such as formaldehyde and the like in the using process, have wide sources and are environment-friendly flame retardant finishing agents.
The sericin used in the invention accounts for 20-30% of the weight of the silk, contains a large amount of amino acids with hydrophilic groups on side chains, such as serine, aspartic acid and the like, and is easy to dissolve in water. The raw materials of the flame retardant used in the invention are waste raw materials in industrial production, can effectively utilize waste such as sericin and the like, changes waste into valuable, and has important significance for environmental protection and resource recycling.
Compared with the traditional layer-by-layer self-assembly technology, the method does not need a large amount of manual operation in the industrial application process, reduces the cross contamination risk among different solutions in the application process, increases the adhesive force of the flame retardant on the surface of the polyester-cotton fabric in a chemical bonding mode, and increases the durability of the flame retardant fabric.
The invention enables the cross-linking complex reaction between the sodium alginate and the metal ions to be generated, the formed cross-linking complex compound increases the carbon forming effect of the polyester-cotton combustion process to a certain extent, the molten drop phenomenon of the polyester-cotton during combustion is slowed down, the combustion process of the polyester-cotton fabric is strengthened from the two aspects of increasing the carbon forming and slowing down the molten drop, and the flame retardant effect of the polyester-cotton fabric is improved to a great extent.
Drawings
FIG. 1 is a chemical bonding process;
FIG. 2 is a schematic diagram of a complexation reaction between metal ions and alginic acid;
FIG. 3 is a vertical combustion diagram of polyester cotton surface coated with different metal ions;
FIG. 4 complex Ca of polyester-cotton2+Vertical combustion patterns before and after the ion water washing;
figure 5 EDS elemental content of fiber surface.
Detailed Description
Examples
The preparation method comprises the steps of preparing the biological hyaluronic acid flame-retardant polyester cotton based on the complexation of reactive sericin and metal ions, and specifically implementing the preparation method by selecting the sericin and alginic acid as flame-retardant finishing agents and the polyester cotton as treated fabrics.
With reference to the attached figures 1-5, putting polyester-cotton in a plasma processor, carrying out plasma treatment on slurry and various additives on the surface of the polyester-cotton for three minutes, then using 5g/L sodium periodate solution to carry out selective oxidation treatment on the surface of the polyester-cotton fabric, using Schiff base reaction to chemically bond 15g/L sericin with the modified polyester-cotton fabric, then further carrying out electrostatic adsorption on the polyester-cotton fabric and a mixed solution of sodium alginate and phytic acid, and spraying Fe with the concentration of 5g/L on the surface of the treated polyester-cotton fabric after drying3+、Mg2+、Cu2+、Ba2+、Co2+、Ni2+Plasma metal ions, so that the loading capacity of the metal ions on the surface of the polyester cotton is 2g/m2The modified polyester cotton is complexed with alginic acid and phytic acid to generate different complex salts, so that the biological hyaluronic acid flame-retardant polyester cotton based on the complexation of the reactive sericin protein and metal ions is prepared.
After various fabrics are subjected to flame retardant treatment, the flame retardant effect is represented by a water washing resistance test, a horizontal combustion test, the front-to-back specific weight of polyester cotton and other test methods.
Table one: proportion, limiting oxygen index and flame retardant grade data of flame retardant finished polyester cotton
And (3) comparing the flame-retardant fabrics subjected to layer-by-layer autonomous assembly and chemical bonding under the same condition, putting polyester-cotton treated by different methods into water, continuously stirring for 30 minutes, putting the polyester-cotton into an oven for drying, testing flame-retardant performance data of different polyester-cotton by using a limit oxygen index meter and a thermogravimetric analyzer for analysis, and comparing the durability of the two treatment modes.
Sodium periodate solutions with different concentrations are taken to carry out oxidation treatment on polyester-cotton fabrics, then the polyester-cotton fabrics are put into 10g/L sericin solution to carry out Schiff base reaction to prepare reactive sericin polyester-cotton fabrics with different oxidation degrees, EDS is used for measuring different nitrogen contents to carry out comparison, and thus the optimal oxidation concentration of the polyester-cotton is determined. Preventing the mechanical structure of the fiber from being damaged by excessive oxidation.
The method comprises the steps of taking the polyester-cotton fabric treated by the same sericin and sodium alginate, then soaking the polyester-cotton fabric in metal ion solutions with different concentrations to perform a complexing reaction, comparing the inhibition degree of the complexing reaction of the metal ions with different concentrations on the polyester-cotton fabric molten drop phenomenon, and measuring the molten drop phenomenon of the polyester-cotton fabric treated by different metal concentrations in a vertical combustion mode. The optimal complexing concentration was found.
The characterization methods referred to in the examples and comparative examples illustrate that:
the surface morphology of the flame-retardant fabric before and after combustion and the product elements before and after combustion were observed by a field emission scanning electron microscope SEM (ULTRA 55, Zeiss, germany).
The limit oxygen index of different metal complex biological hyaluronic acid is measured by a limit oxygen index instrument, so that the flame retardant effect of cotton fabrics treated by different metal ion complex biological hyaluronic acid is judged.
The water resistance and durability of the flame-retardant finishing agent on the surface of the polyester-cotton fabric are measured by a water resistance test. Thus, the adhesion effect of the flame-retardant finishing on the surface of the polyester-cotton fabric is judged.
The surface element content of the polyester-cotton fabric is observed through EDS, so that the optimal oxidation treatment time and the optimal content are determined.
The embodiments only represent a part of the implementation content of the present invention, and are not intended to limit the present invention, and modifications of the technical solutions described in the embodiments or equivalent replacements of part of the technical features may still be included in the scope of the present invention.
Claims (10)
1. A preparation method of biological hyaluronic acid flame-retardant polyester cotton based on reactive sericin and metal ion complexation is characterized by comprising the following steps:
s1, firstly, putting the polyester cotton into a plasma processor to process the surface of the polyester cotton for a certain time, and removing the sizing agent and various additives on the surface of the polyester cotton;
s2, selectively oxidizing the surface of the polyester-cotton fabric by using a strong oxidant solution, chemically bonding sericin with the modified polyester-cotton fabric by using Schiff base reaction, further reacting the polyester-cotton fabric with different biological hyaluronic acids respectively, and finishing the biological hyaluronic acids on the surface of the modified polyester-cotton fabric for later use;
s3, respectively spraying different metal ion solutions on the polyester-cotton fabric manufactured in the S2 to enable the polyester-cotton fabric to be complexed with the biological hyaluronic acid, and thus, the flame-retardant coating polyester-cotton fabric with the reactive sericin and the metal ion complexed biological hyaluronic acid is manufactured.
2. The method for preparing the reactive sericin and metal ion complexing biological hyaluronic acid based flame-retardant polyester cotton according to claim 1, wherein the treatment time of the plasma treatment in the step S1 is 3-20 min.
3. The method for preparing the flame-retardant polyester-cotton fabric based on the reactive sericin and metal ion complexing biological hyaluronic acid according to claim 1, wherein in the step S1, the content of the polyester in the polyester-cotton fabric is 5% -100%.
4. The method for preparing the flame-retardant polyester cotton based on the reactive sericin and metal ion complexing biological hyaluronic acid according to any one of claims 1 to 3, wherein the strong oxidant is one or more of sodium periodate, sodium hypochlorite and hydrogen peroxide in step S2.
5. The method for preparing the flame-retardant polyester cotton based on the reactive sericin and metal ion complexing biological hyaluronic acid according to claim 4, wherein the concentration of the strong oxidant solution in the step S2 is 5g/L-20 g/L.
6. The method for preparing the flame-retardant polyester cotton based on the reactive sericin and metal ion complexing biological hyaluronic acid according to claim 4, wherein in the step S2, the content of sericin is 10-100 g/L. The loading capacity on the surface of the polyester-cotton fabric is 20-60g/m2。
7. The method for preparing the flame-retardant polyester cotton based on the reactive sericin and metal ion complexing biological hyaluronic acid according to claim 4, wherein in the step S2, the content of the aqueous solution of the biomass acid is 1g/L-10 g/L. The loading capacity on the surface of the polyester-cotton fabric is 1-10g/m2。
8. The method for preparing the flame-retardant polyester cotton based on the reactive sericin complex with the biological hyaluronic acid as defined in any one of claims 5 to 7, wherein the biological hyaluronic acid is one or more of alginic acid, tannin and phytic acid in step S2.
9. The method for preparing the biological acid flame-retardant polyester cotton based on the complexation of the reactive sericin protein and the metal ions according to claim 1, wherein in the step S3, the different metal ions comprise: fe3+、Mg2+、Cu2+、Ba2+、Co2+、Ni2 +One or more of plasma metal ions, wherein the concentration of the metal ion solution is 1g/L-10g/L, and the spraying amount of the metal ion solution is 1g/m2-10g/m2。
10. A biological hyaluronic acid flame-retardant polyester cotton based on complexation of reactive sericin protein and metal ions, which is characterized by being prepared by the method of any one of claims 1-9.
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