阅读说明：本技术 一种防辐射纤维及其制备方法和防护服 (Radiation-proof fiber, preparation method thereof and protective clothing ) 是由 徐开玖 张茂青 马玲玲 汤飞辉 缪夕霞 林磊 于 2021-06-30 设计创作，主要内容包括：本申请涉及防辐射材料的技术领域,更具体地说,它涉及一种防辐射纤维及其制备方法和防护服。防辐射纤维由包含以下重量份的原料制成：50-90份纤维素黄酸酯以及2-10份纳米金属粉末以及10-20份稀氢氧化钠水溶液,且所述纳米金属粉末为纳米银粉末、纳米氧化锌粉末以及纳米硫酸钡粉末中的一种或者几种的组合物；其制备方法为：(1)制备粘胶原液；(2)制备纺丝原液；(3)制备防辐射粗纤维；(4)制备防辐射纤维。本申请的防辐射纤维及其制备方法均具有保持防护服的防辐射性能并提升其舒适度的效果。(The application relates to the technical field of radiation-proof materials, in particular to radiation-proof fibers, a preparation method thereof and protective clothing. The radiation-proof fiber is prepared from the following raw materials in parts by weight: 50-90 parts of cellulose xanthate, 2-10 parts of nano metal powder and 10-20 parts of dilute sodium hydroxide aqueous solution, wherein the nano metal powder is one or a combination of nano silver powder, nano zinc oxide powder and nano barium sulfate powder; the preparation method comprises the following steps: (1) preparing a viscose stock solution; (2) preparing a spinning solution; (3) preparing radiation-proof coarse fibers; (4) and preparing the radiation-proof fiber. The radiation-proof fiber and the preparation method thereof have the effects of keeping the radiation-proof performance of the protective clothing and improving the comfort level of the protective clothing.)

1. The radiation-proof fiber is characterized by being prepared from the following raw materials in parts by weight: 50-90 parts of cellulose xanthate, 2-10 parts of nano metal powder and 10-20 parts of dilute sodium hydroxide aqueous solution, wherein the nano metal powder is one or a combination of nano silver powder, nano zinc oxide powder and nano barium sulfate powder.

2. The radiation protective fiber of claim 1 wherein: the feed is prepared from the following raw materials in parts by weight: 65-75 parts of cellulose xanthate, 5-7 parts of nano metal powder and 13-17 parts of dilute sodium hydroxide aqueous solution.

3. The radiation protective fiber of claim 1 wherein: the particle size of the nano metal powder is between 30 and 80 nm.

4. The radiation protective fiber of claim 1 wherein: the pH value of the dilute sodium hydroxide aqueous solution is between 7.5 and 9.5.

5. The radiation protective fiber of claim 1 wherein: the radiation-proof fabric also comprises 5-15 parts of radiation-proof additive, wherein the radiation-proof additive is one or a mixture of more of bee venom titanium, pearl powder and catalase.

6. The radiation protective fiber of claim 5 wherein: the radiation-proof additive is a mixture of bee venom titanium, pearl powder and catalase, and the weight ratio of the bee venom titanium to the pearl powder to the catalase is 1:1: 3.

7. The radiation protective fiber of claim 5 wherein: the nano metal powder is a mixture of nano silver powder and nano zinc oxide powder, and the weight ratio of the nano silver powder to the nano zinc oxide powder is 4: 1.

8. A method of making radiation protective fibers of any of claims 1-7 comprising the steps of:

(1) sequentially adding cellulose xanthate and nano metal powder into a dilute sodium hydroxide aqueous solution, and then stirring and mixing to obtain a viscose stock solution;

(2) standing the viscose fiber stock solution at the temperature of 30-60 ℃, and then washing to be neutral to obtain a spinning stock solution;

(3) spinning the spinning solution, and obtaining radiation-proof crude fiber through a coagulating bath;

(4) and (3) carrying out water washing, desulfurization and drying on the radiation-proof coarse fiber to obtain the radiation-proof fiber.

9. Protective clothing, characterized in that it is woven from the radiation protective fibres according to claims 1-7.

Technical Field

The application relates to the technical field of radiation-proof materials, in particular to radiation-proof fibers, a preparation method thereof and protective clothing.

Background

Electromagnetic radiation is an invisible and untouchable pollution known as "invisible killer". Most household appliances such as televisions, microwave ovens and shavers contacted by people in daily life can generate electromagnetic radiation in various forms, and the electromagnetic radiation has direct or indirect damage to human reproductive systems, nervous systems and immune systems, and particularly for pregnant women, the possibility of causing pathological changes such as abortion, sterility, teratogenesis and the like exists.

In the related art, in order to reduce the damage of electromagnetic radiation to the pregnant woman, the silver fiber and the pure cotton fiber are blended to obtain the protective clothing, so that when the pregnant woman wears the protective clothing, the protective clothing can form a protective cover for shielding the electromagnetic radiation through the silver fiber, and then the electromagnetic radiation protection of the pregnant woman is completed.

In view of the above-mentioned related arts, the inventors believe that, although the protective clothing made of silver fibers and pure cotton fibers has extremely excellent radiation shielding performance, the surface of the silver fibers may have some fine burrs, so that when a pregnant woman wears the protective clothing close to the skin in a hot weather environment, the fine burrs easily damage the skin of the pregnant woman, and the protective clothing has a defect of poor comfort.

Disclosure of Invention

In order to improve the comfort level of protective clothing, the application provides radiation-proof fibers, a preparation method of the radiation-proof fibers and the protective clothing.

In a first aspect, the present application provides a radiation protective fiber, which adopts the following technical scheme:

the radiation-proof fiber is prepared from 50-90 parts by weight of cellulose xanthate, 2-10 parts by weight of nano metal powder and 10-20 parts by weight of dilute sodium hydroxide aqueous solution, wherein the nano metal powder is one or a combination of nano silver powder, nano zinc oxide powder and nano barium sulfate powder.

By adopting the technical scheme, as nano metal powder such as nano silver powder, nano zinc oxide powder and nano barium sulfate powder is adopted as the radiation-proof metal material, and cellulose xanthate is adopted as the fiber base material, so that the cellulose xanthate can be used as a carrier to force the nano metal powder to be connected with each other, and further, when the generation of burrs of the radiation-proof fiber is reduced and the comfort level of the protective clothing is improved, a protective cover for shielding electromagnetic radiation can be formed as well, and the radiation-proof effect is obtained.

In addition, as the cellulose xanthate is used as the fiber base material to load the nano metal powder, and the cellulose xanthate can be used for preparing the ice silk fiber with excellent comfort, the comfort of the protective clothing is further improved.

In addition, because the dilute sodium hydroxide aqueous solution is used as the solvent, the nano metal powder can be more uniformly dispersed in the cellulose xanthate, and the radiation-proof performance of the radiation-proof fiber is further improved.

Preferably, the feed additive is prepared from the following raw materials in parts by weight: 65-75 parts of cellulose xanthate, 5-7 parts of nano metal powder and 13-17 parts of dilute sodium hydroxide aqueous solution.

By adopting the technical scheme, due to the adoption of the cellulose xanthate, the nano metal powder and the dilute sodium hydroxide aqueous solution in the proportion, the nano metal powder can be more easily dispersed in the cellulose xanthate through the dilute sodium hydroxide aqueous solution, and the radiation-proof performance of the radiation-proof fiber is effectively improved.

Preferably, the particle size of the nano metal powder is between 30 and 80 nm.

By adopting the technical scheme, as the nano metal powder within the particle size range is adopted, when the pregnant woman wears the protective clothing woven by the radiation-proof fibers, the quantity of the radiation-proof fibers can be effectively reduced

The possibility of a reduction in the comfort of the protective garment due to the larger nano-metal powder particles.

In addition, due to the adoption of the nano metal powder in the particle size range, the possibility that thixotropy is caused due to small particle size and the viscosity is increased suddenly can be effectively reduced, and the operation difficulty for preparing the radiation-proof fiber is indirectly reduced.

Preferably, the pH value of the dilute aqueous sodium hydroxide solution is between 7.5 and 9.5.

By adopting the technical scheme, due to the adoption of the pH value within the range, the cellulose xanthate is effectively dissolved by the dilute sodium hydroxide aqueous solution, the nanometer metal powder is more uniformly dispersed in the cellulose xanthate, the possibility of denaturation of the cellulose xanthate caused by overhigh alkalinity of the dilute sodium hydroxide aqueous solution can be effectively reduced, and the radiation protection performance of the radiation protection fiber is indirectly improved.

Preferably, the radiation-proof fabric also comprises 5-15 parts of radiation-proof additive, wherein the radiation-proof additive is one or a mixture of more of bee venom titanium, pearl powder and catalase.

By adopting the technical scheme, the bee venom titanium, the pearl powder and the catalase are used as the radiation-proof additives and added into the radiation-proof fiber system, so that the bee venom titanium, the pearl powder and the catalase can regulate the neuroendocrine of a human body and remove free radicals in the human body while the radiation-proof performance of the radiation-proof fiber is improved, and further the radiation resistance of the human body is effectively improved.

Preferably, the radiation-proof additive is a mixture of bee venom titanium, pearl powder and catalase, and the weight ratio of the bee venom titanium, the pearl powder and the catalase is 1:1: 3.

By adopting the technical scheme, the radiation resistance of the human body can be further improved while the radiation resistance of the radiation-proof fiber is further improved due to the adoption of the bee venom titanium, the pearl powder and the catalase in the proportion.

Preferably, the nano metal powder is a mixture of nano silver powder and nano zinc oxide powder, and the weight ratio of the nano silver powder to the nano zinc oxide powder is 4: 1.

By adopting the technical scheme, the nano silver powder and the nano zinc oxide powder in the proportion are adopted, so that the nano silver powder and the nano zinc oxide powder can effectively improve the activity of catalase and further improve the radiation resistance of a human body while further improving the radiation resistance of the radiation-proof fiber.

In a second aspect, the application provides a preparation method of radiation-proof fiber, which adopts the following technical scheme:

a preparation method of radiation-proof fiber comprises the following steps:

(1) sequentially adding cellulose xanthate and nano metal powder into a dilute sodium hydroxide aqueous solution, and then stirring and mixing to obtain a viscose stock solution;

(2) standing the viscose fiber stock solution at the temperature of 30-60 ℃, and then washing to be neutral to obtain a spinning stock solution;

(3) spinning the spinning solution, and obtaining radiation-proof crude fiber through a coagulating bath;

(4) and (3) carrying out water washing, desulfurization and drying on the radiation-proof coarse fiber to obtain the radiation-proof fiber.

By adopting the technical scheme, in the step (2), because the viscose stock solution is kept stand at the temperature for the time, the esterification degree of the cellulose xanthate is effectively reduced, the viscosity and the stability of the viscose stock solution are adjusted, and the radiation-proof performance of the radiation-proof fiber can be indirectly improved while the operation difficulty of preparing the radiation-proof fiber is effectively reduced.

In a third aspect, the present application provides a protective garment, which adopts the following technical scheme:

a protective garment is woven from the radiation-proof fiber.

In summary, the present application has the following beneficial effects:

1. because this application adopts nanometer metal powder as anti-radiation metal material, adopts cellulose xanthate as the fibre base material, and then when reducing the production of the fibrous burr of protecting against radiation and improving the comfort level of protective clothing, can also impel the fibrous effect that obtains protecting against radiation of protecting against radiation.

2. The cellulose xanthate is preferably adopted as the fiber base material to load the nano metal powder, and the cellulose xanthate can be used for preparing the ice silk fiber with excellent comfort, so that the effect of further improving the comfort of the protective clothing is obtained.

3. According to the method, the radiation-proof fiber is kept stand at the temperature of 30-60 ℃, so that the effects of reducing the operation difficulty of preparing the radiation-proof fiber and indirectly improving the radiation-proof performance of the radiation-proof fiber are achieved.

Drawings

FIG. 1 is a flow chart of a method of making radiation protective fibers provided herein.

Detailed Description

The present application will be described in further detail with reference to examples and comparative examples.

Raw materials

The raw material components in the application are shown in a table 1:

TABLE 1 sources of the raw material components

Examples

Example 1

A radiation-proof fiber is prepared by the following steps:

(1) 70kg of cellulose xanthate and 6kg of nano-silver powder (particle size 55nm) were sequentially added to 15kg of 16% aqueous sodium hydroxide solution (pH 8.5), followed by mixing at a stirring speed of 500r/min for 1h to obtain a viscose dope;

(2) standing the viscose fiber stock solution at the temperature of 45 ℃ for 6 hours, and then washing the viscose fiber stock solution to be neutral by using deionized water to obtain spinning stock solution;

(3) spinning the spinning stock solution, and carrying out coagulation bath on the spinning stock solution through a saturated zinc sulfate solution to obtain radiation-proof crude fiber;

(4) and (3) washing the radiation-proof crude fiber in deionized water, desulfurizing through poly hexanediol dimethyl ether, and finally drying by natural blowing to obtain the radiation-proof fiber.

Examples 2 to 9

The differences from example 1 are that the weights of the cellulose xanthate, the nano silver powder and the 16% aqueous sodium hydroxide solution in examples 2 to 9 are different, as shown in table 2.

TABLE 2 compositions of the materials of examples 1-9 and weight tables (kg)

Example 10

The difference from example 1 is that the nano silver powder has a particle size of 30 nm.

Example 11

The difference from example 1 is that the nano silver powder has a particle size of 80 nm.

Example 12

The difference from example 1 is that the pH of the 16% aqueous sodium hydroxide solution was 9.5.

Example 13

The difference from example 1 is that the pH of the 16% aqueous sodium hydroxide solution was 7.5.

Example 14

The difference from the example 1 is that (1) also comprises 10kg of bee venom titanium.

Example 15

The difference from example 14 is that the weight of titanium bee venom was 15 kg.

Example 16

The difference from example 14 is that the weight of melittin is 5 kg.

Example 17

The difference from example 14 is that titanium bee venom was replaced with pearl powder of the same weight.

Example 18

The difference from example 14 was that titanium bee venom was replaced with catalase in the same weight.

Example 19

The difference from example 14 was that the melittin was replaced with a mixture of catalase and melittin in the same weight ratio of catalase to melittin of 1: 1.

Example 20

The difference from example 14 is that the bee venom titanium was replaced with a mixture of catalase and pearl powder in the same weight ratio of catalase to pearl powder of 1: 1.

Example 21

The difference from example 14 was that the melittin was replaced with a mixture of catalase, pearl powder and melittin in the same weight ratio of catalase, pearl powder and melittin of 1:1: 1.

Example 22

The difference from example 21 was that the melittin was replaced with a mixture of catalase, pearl powder and melittin in the same weight ratio of catalase, pearl powder and melittin of 1:1: 5.

Example 23

The difference from example 21 was that the melittin was replaced with a mixture of catalase, pearl powder and melittin in the same weight ratio of catalase, pearl powder and melittin of 1:1: 3.

Example 24

The difference from example 23 is that nano silver powder was replaced with nano barium sulfate powder of the same weight.

Example 25

The difference from example 23 is that nano silver powder was replaced with nano zinc oxide powder of the same weight.

Example 26

The difference from example 23 is that the nano silver powder was replaced with a mixture of nano silver powder and nano zinc oxide powder in the same weight ratio of 1: 1.

Example 27

The difference from example 23 is that the nano silver powder was replaced with a mixture of nano silver powder and nano zinc oxide powder in the same weight ratio of 4: 1.

Example 28

The difference from example 23 is that the nano silver powder was replaced with a mixture of nano silver powder and nano zinc oxide powder in the same weight ratio of 3: 1.

Example 29

The difference from example 27 is that in (2), the viscose dope is left to stand at a temperature of 30 ℃ for 6 h.

Example 30

The difference from example 27 is that in (2), the viscose dope is left to stand at a temperature of 70 ℃ for 6 h.

Comparative example

Comparative example 1

The difference from example 1 is that a 16% aqueous solution of sodium hydroxide was not included.

Application examples

Application examples 1 to 30

A protective garment woven from the radiation protective fibers of examples 1-28.

Comparative application

Application comparative example 1

A protective garment is prepared by blending silver fiber and pure cotton fiber.

Comparative application example 2

The difference from application example 1 is that the radiation protective fiber of comparative example 1 is woven.

Performance test

Test method

Three samples were taken from application examples 1 to 30 and application comparative examples 1 to 2, respectively, and then cut into protective cloths of the same shape, and finally the following tests were performed and averaged.

Test one, comfort detection

The samples were placed on the same plane and subsequently evaluated by fifty evaluators, and comfort to the samples was expressed as "Sa" according to a minority majority-compliant principle.

Sa0, smooth and without roughness;

sa 1: a rough feel;

sa 2: has rough feeling;

sa 3: has stabbing pain.

Test two, radiation protection detection

The samples were used to coat a razor, and the radiation values were measured ten times with the razor open by an electromagnetic radiation tester and averaged. It should be noted that, in the present application, the average value of the radiation of the shaver without any sample is 19.62ut, and the national safety radiation standard is less than 0.2 ut.

And (3) detection results: the results of the tests of practical examples 1 to 30 and practical comparative examples 1 to 2 are shown in Table 3.

TABLE 3 tables of test results of application examples 1 to 30 and application comparative examples 1 to 2

In the combination of application examples 1 to 5 and application comparative example 1 and in combination with table 3, it can be seen that, although the radiation values of application examples 1 to 5 are improved compared with application comparative example 1, the radiation values of application examples 1 to 5 are still under the national safety standard, and the comfort levels of application examples 1 to 5 are all obviously improved. Particularly, in the application example 1, the comfort level is relatively optimal under the premise of a low radiation value, so that the cellulose xanthate and the nano silver powder are superior in the specific gravity of the application example 1.

In combination with application example 1, application examples 6 to 9, and application comparative example 2, and in combination with table 3, it can be seen that, compared to application example 1, the radiation values of application example 6 and application example 8 are still below the national safety standard, but the radiation values are improved. While the comfort degree is greatly deteriorated by applying the comparative example 2, the radiation value even exceeds the national safety standard, so that the 16% sodium hydroxide aqueous solution has great effect on the radiation protection performance and the comfort degree of the protective clothing.

However, the comfort and the radiation value of application example 1 were not significantly changed from those of application examples 7 and 9, and the specific gravity of application example 1 was still superior for cost.

As can be seen by combining application example 1, application examples 10 to 11, and application comparative example 1, and combining table 3, although the radiation protection performance and the comfort level of application examples 10 to 11 are not much different from those of application comparative example 1, it is demonstrated that the particle size of the nano silver powder is within the range of examples 10 to 11, and the radiation protection performance and the comfort level of the protective clothing can be improved.

Although the radiation protection performance of the application examples 10 to 11 is not significantly changed compared to the application example 1, the comfort of the application example 10 is significantly deteriorated, and the application example is too high in cost and also high in preparation difficulty, so that the application example 1 is still better.

As can be seen by combining application example 1, application examples 12 to 13, and application comparative example 1 with table 3, although the radiation protection performance and the comfort level of application examples 12 to 13 are not much different from those of application comparative example 1, it is demonstrated that the pH of the 16% aqueous sodium hydroxide solution is within the range of examples 12 to 13, and the radiation protection performance and the comfort level of the protective clothing can be improved. However, the radiation protection performance of each of the application examples 12 to 13 was reduced compared to that of the application example 1, and therefore, the application example 1 was still superior.

As can be seen from the combination of application example 1, application examples 14 to 16, and table 3, compared with application example 1, the radiation protection performance of application examples 14 to 16 is significantly improved, which indicates that melittin has the effect of improving the radiation protection performance of the protective clothing.

Particularly, in the application examples 14 to 15, the effect of improving the radiation protection performance is the best. However, the amount of melittin added in application example 14 was relatively small compared to application example 15, and thus application example 14 was preferable.

In combination with application example 1, application example 14, and application examples 17 to 18, and in combination with table 3, it can be seen that the radiation protection performance of application examples 17 to 18 is improved compared to application example 1, and thus, the pearl powder and catalase also have the effect of improving the radiation protection performance of the protective clothing, and the improvement effect of catalase is the best.

It can be seen from the combination of application example 14 and application examples 19 to 23 and the combination of table 3 that, compared with application example 14, the radiation protection performance of application examples 19 to 23 is significantly improved, and particularly the improvement effect of application example 23 is the best, so that when the melittin, the pearl powder and the catalase are used cooperatively, the radiation protection performance of the protective clothing can be further improved, and the improvement effect is the best when the proportion of application example 23 is used cooperatively.

As can be seen from the combination of application examples 23 to 25 and table 3, compared with application example 23, the radiation protection performance of application examples 24 to 25 is not greatly reduced, which shows that the nano barium sulfate powder and the nano zinc oxide powder also have a certain effect of improving the radiation protection performance of the protective clothing, and the nano zinc oxide powder may have an effect of improving the enzyme activity, and the improvement effect is slightly worse than that of the nano silver powder, but the cost is lower.

It can be seen from the combination of application example 23, application examples 26 to 28 and table 3 that the radiation protection performance of application examples 26 to 28 is only slightly reduced compared to that of example 23, and even the radiation protection performance of application example 27 is the same as that of application example 23, thereby illustrating that when the nano silver powder is compounded with the nano zinc oxide powder, especially within the proportion range of application example 27, the same improvement effect as that of pure nano silver powder can be achieved, and for cost, application example 27 is better.

As can be seen from the combination of application example 27, application examples 29 to 30 and table 3, the radiation protection performance of application examples 29 to 30 is significantly reduced compared to application example 27, which shows that the standing temperature has a significant effect on the radiation protection performance of the protective clothing, and thus application example 27 is still superior.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.