阅读说明：本技术 一种光催化马来酸酐接枝亚麻布的方法 (Method for grafting linen with maleic anhydride through photocatalysis ) 是由 孙才英 苟巧林 李燕 任彪彪 李宏章 杨娅 迭恺 于 2019-10-15 设计创作，主要内容包括：一种光催化马来酸酐接枝亚麻布的方法,涉及复合材料制备领域,具体方案如下：一种光催化马来酸酐接枝亚麻布的方法,包括如下步骤：步骤一、将亚麻布放入16％的氢氧化钠水溶液中30s取出,用蒸馏水洗涤至中性,放入真空干燥箱中烘干；步骤二、将烘干后的亚麻布放在含有光催化剂的马来酸酐溶液中浸泡15min取出,然后每一面亚麻布照射紫外光2-4min；步骤三、照射完成之后,取出亚麻布,用蒸馏水洗涤至中性,放入真空干燥箱中干燥得到已接枝马来酸酐的亚麻布。紫外光催化光接枝法,在亚麻布表面接枝马来酸酐,克服了传统熔融法和溶液法的耗能高、工艺复杂、污染大等缺点,工艺简单,接枝率高。(A method for grafting linen with maleic anhydride by photocatalysis relates to the field of composite material preparation, and the specific scheme is as follows: a method for grafting linen with maleic anhydride under photocatalysis comprises the following steps: step one, putting linen into a 16% sodium hydroxide aqueous solution for 30s, taking out, washing the linen to be neutral by using distilled water, and putting the linen into a vacuum drying oven for drying; secondly, soaking the dried linen in a maleic anhydride solution containing a photocatalyst for 15min, taking out, and then irradiating each surface of the linen with ultraviolet light for 2-4 min; and step three, after the irradiation is finished, taking out the linen, washing the linen to be neutral by using distilled water, and drying the linen in a vacuum drying oven to obtain the linen grafted with maleic anhydride. The ultraviolet light catalysis light grafting method grafts maleic anhydride on the surface of the linen, overcomes the defects of high energy consumption, complex process, large pollution and the like of the traditional melting method and solution method, and has simple process and high grafting rate.)

1. A method for grafting linen by maleic anhydride through photocatalysis is characterized in that: the method comprises the following steps:

step one, putting linen into a 16% sodium hydroxide aqueous solution for 30s, taking out, washing the linen to be neutral by using distilled water, and putting the linen into a vacuum drying oven for drying;

secondly, soaking the dried linen in a maleic anhydride solution containing a photocatalyst for 15min, taking out, and then irradiating each surface of the linen with ultraviolet light for 2-4 min;

and step three, after the irradiation is finished, taking out the linen, washing the linen to be neutral by using distilled water, and drying the linen in a vacuum drying oven to obtain the linen grafted with maleic anhydride.

2. The method of claim 1, wherein the method comprises the steps of: in the first step, the drying temperature is 60 ℃ and the drying time is 90 min.

3. The method of claim 1, wherein the method comprises the steps of: in the second step, the solvent of the maleic anhydride solution is N, N-dimethylformamide solution DMF.

4. A method of photocatalytic maleic anhydride grafted linen as claimed in claim 1 or 3, characterized in that: in the second step, the mass concentration of the maleic anhydride in the maleic anhydride solution is 10-50%.

5. The method of claim 1, wherein the method comprises the steps of: in the second step, the photocatalyst is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide.

6. The method of claim 1, wherein the method comprises the steps of: in the second step, the mass of the photocatalyst is 2% of the mass of the weighed maleic anhydride.

7. The method of claim 1, wherein the method comprises the steps of: in the second step, the power of the ultraviolet lamp for irradiating the ultraviolet light is 112-280w, and the wavelength is 395 nm.

8. The method of claim 1, wherein the method comprises the steps of: in the third step, the drying temperature is 60 ℃ and the drying time is 90 min.

Technical Field

The invention relates to the field of composite material preparation, in particular to a method for grafting linen with maleic anhydride by photocatalysis.

Background

The prior maleic anhydride grafting method comprises thermal grafting, photo-grafting, radiation grafting and other methods according to different free radical initiation modes^[1](ii) a According to the state of natural fibre, there are solution method, melting method and solid phase method.

Solution grafting method^[1]The recovery is troublesome, the production cost is high, and the used organic solvent can cause harm to human bodies and damage to the environment. And the grafted fiber needs to be drawn again to weave the linen.

Melt grafting process^[2]The method has the characteristics of simple operation, low cost, suitability for industrial production and the like, but the method has high reaction temperature, so that the natural fibers are seriously degraded, and the mechanical property of the matrix is reduced. The grafted fiber needs to be drawn again to weave linen.

The hot grafting method generally adopts grafting at a certain temperature, has higher requirements on the temperature, is easy to denature in the reaction for materials with lower melting points or poor stability, and is not suitable for linen.

Radiation grafting method^[3]-[4]High-price equipment is needed to generate high-energy rays, and the method is easy to damage the base material, so that the method is not suitable for industrial continuous production.

Jun Qian^[5]The Maleic Anhydride (MAH) is grafted to the PP by three grafting modes of ultrasonic wave, high-energy ray radiation and co-radiation of the ultrasonic wave and the high-energy ray radiation, the influence of different co-monomers on the grafting rate is compared and researched, and the method is high in energy consumption. The greatest disadvantage of radiation grafting is that homopolymerization of the monomers inevitably occurs when the polymer monomer mixed system is irradiated simultaneously, which reduces grafting efficiency and increases the step of removing the homopolymer.

The references are as follows:

[1] ginger great labra, Xuqingling, nabusao, Wanyangbei, grandsbury, Sun Caiying, Na- + flame retardant modified flax fiber and the influence on the fiber performance [ J ] fine chemical industry, 2019,36(09):1809-1815.

[2] Very gorgeous, sheddown, popalashu, et al comparison of polypropylene melt-grafted and pre-irradiated grafted maleic anhydride [ J ] plastics industry, 2016,44(6):41-45.

[3] Research on gamma-ray radiation grafting of methyl acrylate on ultra-high molecular weight polyethylene fibers [ J ] 2011.

[4] Preparation and characterization of Wangfeng, Tongbin, Polypropylene radiation grafting silane [ J ] radiation research and radiation technology bulletin, 2009,27(5):261 wall 264.

[5]Qian Jun,Huang Zhijuan,Dang Shuaiying,etal.Improvements ofpolypropylene grafted maleic anhydridewith untrasonication,pre-irradiationand co-irradiation methods[J].Journal ofPolymer Research,2011,18(1):1557-1565.

Disclosure of Invention

The invention aims to provide a method for grafting maleic anhydride onto linen through photocatalysis by ultraviolet light, introduce double bonds and carboxyl functional groups, and further perform modification such as flame retardance, electric conduction and the like on the linen according to needs.

The natural linen has the advantages of air permeability, antibiosis, wear resistance and the like, and is commonly used for decorative materials of clothes, houses, vehicles, ships, airplanes and the like. Linen is not conductive by itself.

In order to achieve the purpose, the invention adopts the following technical scheme:

a method for grafting linen with maleic anhydride under photocatalysis comprises the following steps:

step one, putting linen into a 16% sodium hydroxide aqueous solution for 30s, taking out, washing the linen to be neutral by using distilled water, and putting the linen into a vacuum drying oven for drying;

secondly, soaking the dried linen in a maleic anhydride solution containing a photocatalyst for 15min, taking out, and then irradiating each surface of the linen with ultraviolet light for 2-4 min;

and step three, after the irradiation is finished, taking out the linen, washing the linen to be neutral by using distilled water, and drying the linen in a vacuum drying oven to obtain the linen grafted with maleic anhydride.

Further, in the step one, the drying temperature is 60 ℃, and the drying time is 90 min.

Further, in the second step, the solvent of the maleic anhydride solution is N, N-Dimethylformamide (DMF).

Further, in the second step, the mass concentration of the maleic anhydride in the maleic anhydride solution is 10-50 wt%.

Further, in the second step, the photocatalyst is 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide.

Further, in the second step, the mass of the photocatalyst is 2% of the mass of the weighed maleic anhydride.

Further, the power of the ultraviolet lamp irradiating the ultraviolet light in the second step is 112-.

Further, in the third step, the drying temperature is 60 ℃, and the drying time is 90 min.

The invention has the beneficial effects that:

(1) the ultraviolet light catalysis light grafting method grafts maleic anhydride on the surface of the linen, overcomes the defects of high energy consumption, complex process, large pollution and the like of the traditional melting method and solution method, has simple process and high grafting rate, and the grafting rate can reach 62.11 percent under the conditions that the mass concentration of the maleic anhydride is 40 percent and the irradiation time is 4min on the front side and the back side respectively.

(2) Ultraviolet light has less penetration to the material than high-energy radiation, so that graft polymerization can be strictly limited to the surface or subsurface of the material without damaging the bulk properties of the material.

(3) The light source of ultraviolet radiation and the equipment thereof have low cost, the reaction degree is easy to control, and the continuous industrial production is easy to realize; meanwhile, the photo-grafting is an environment-friendly green grafting technology, has the advantages of low polymerization energy consumption, high polymerization speed, high production efficiency, low polymerization reaction temperature, simple reaction equipment, small environmental pollution and the like, and conforms to the concept of green environmental chemistry.

Drawings

FIG. 1 is an infrared spectrum of linen before and after grafting, wherein the ordinate is absorbance in%, and the abscissa is absorption wavelength in cm^-1。

Detailed Description

The technical solution of the present invention is further described with reference to fig. 1 and the detailed description, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.