CN102922538A - Method for producing tritium-proof gloves - Google Patents

Method for producing tritium-proof gloves Download PDF

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CN102922538A
CN102922538A CN2012104209708A CN201210420970A CN102922538A CN 102922538 A CN102922538 A CN 102922538A CN 2012104209708 A CN2012104209708 A CN 2012104209708A CN 201210420970 A CN201210420970 A CN 201210420970A CN 102922538 A CN102922538 A CN 102922538A
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layer
hydrogen
tritium
step
mold
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CN2012104209708A
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CN102922538B (en
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帅茂兵
郑少涛
罗晓娜
张广丰
杨喜梅
汪小琳
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四川材料与工艺研究所
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Abstract

The invention provides a method for producing a pair of tritium-proof gloves and belongs to the field of a radiation proof material. The method comprises the step of: preparing a three-layer compound rubber thin film by using a method of compounding layer by layer, wherein the outer layer is a rubber barrier layer which is good in hydrogen stopping property; the middle layer is a tritium absorption layer in which an organic hydrogen absorption agent prepared by DEB and a catalyst is dispersed; and the third layer is a rubber layer which is good in compatibility with the skin and is made of the same material as the outer layer. The gloves produced by using the method has the advantages that tritium permeating into each tritium-proof glove through surface layer rubber is fixed in the rubber layer of the middle layer of each glove, thereby achieving the tritium-proof effect; and the preparation process is simple, the tritium-proof effect is obvious and the tritium recycle and the environmental protection can be realized.

Description

一种防氚手套的制备方法 A method of preparing anti-tritium glove

技术领域 FIELD

[0001] 本发明涉及一种防辐射材料的制作,特别是涉及一种用于防氚手套的材料的制备方法。 [0001] The present invention relates to a radiation protection material production, in particular, relates to a material for tritium gloves preparation.

背景技术 Background technique

[0002] 在氚操作中离不开手套箱,手套箱相对开放的位置就是手套。 [0002] In a glove box inseparable tritium operation, the glove box is relatively open position of the glove. 手套也是操作人员最接近氚的地方。 Gloves also the place where people closest to the tritium operation. 防氚手套多采用高分子材料,氚在高分子材料中的渗透以及长期暴露于辐射环境下都会导致材料性能的下降。 Tritium gloves to use more polymer materials, tritium permeation in polymer materials and long-term exposure to radiation environment will lead to a decline material properties. 因此,研制氚防护高分子材料一般需要解决以下问题:减缓氚在材料中的渗透,增强材料的抗β粒子辐射性能,降低辐照和氚与材料作用后产生的化学腐蚀,降低氢同位素交换的可能性。 Therefore, the development of polymer materials generally require protection tritium address the following issues: slowed tritium permeation in the material, particulate material to enhance the anti-β radiation performance, reduce chemical corrosion and tritium produced after irradiation and effect materials, the reduction of hydrogen isotope exchange possibility. 目前使用的防氚手套都是使用具有良好的抗氚辐照性能以及阻氚性能的丁基橡胶等来制备。 Currently tritium were used to prepare gloves having good anti-blocking properties and tritium tritium radiation performance butyl rubber.

[0003] 在防氚手套结构方面,根据材料的不同特性而进行材料的多层优化组合是防氚手套研究的一个较好的思路。 [0003] In terms of structure tritium gloves, depending on the characteristics of the material of the multilayer optimized combination of materials is a good idea studies tritium gloves. 如武可迁以丁基橡胶、硅橡胶为主体材料,添加防渗透剂,并外覆金属薄膜,研制出5层材质复合结构防氚手套,具有较好的防氚效果(氚防护手套的研制与应用,1990,37)。 The Transitive Wu butyl rubber, silicone rubber as the main material, adding penetration inhibitor, and a metal thin film overcoat, developed a five-layer composite structure tritium glove material, has good effect developed tritium (tritiated protective gloves and applications, 1990,37). 但是现有技术中提到的防氚手套虽然采用了5层复合结构,但各层的作用均是通过物理隔离的方式来防止氚的渗透,这也是传统的防氚手套防止氚渗透的方法。 However, the prior art gloves tritium mentioned although the use of five-layer composite structure, but the role of each layer are to prevent the penetration of tritium through physically isolated manner, which is the traditional method of tritium permeation of tritium gloves prevented. 通过物理隔离的方式制作的防氚手套,随着时间的推移,氚总会渗透到操作者一侧,从而伤害操作者和污染环境,也同时造成了氚的损失。 Produced by physically isolated manner tritium gloves, over time, to tritium permeation operator side always, so that injury to the operator and environmental pollution, and also resulted in the loss of tritium.

发明内容 SUMMARY

[0004] 本发明的目的是解决现有技术的问题,提供一种防氚手套的制备方法,该方法制作的手套将通过表层橡胶渗透到防氚手套中的氚固定在手套中间层的胶层中来达到防氚的效果,制备工艺简单,防氚效果显著且有利于氚回收及环境保护。 [0004] The object of the present invention is to solve the problems of the prior art, there is provided a method of preparing tritium gloves, the gloves made by the method to tritium permeation of tritium fixed subbing layer glove in the glove surface by a rubber intermediate layer to achieve the effect of tritium in the preparation process is simple, the effect is significant tritium and tritium facilitate recovery and environmental protection.

为达到上述目的,本发明采用的技术方案是:一种防氚手套的制备方法,制作具有三层结构的防氚手套,即第一层阻氢层、第二层吸氢层和第三层阻氢层,具体步骤包括: To achieve the above object, the technical solution of the present invention is that: a method of preparing tritium gloves, glove tritium produced having three-layer structure, i.e., a first layer of a hydrogen barrier layer, a second layer and a third layer absorbing layer a hydrogen barrier layer, the specific steps include:

步骤一:制备吸氢剂,按照质量比3:1的比例将DEB和碳催化剂粉末混合,放入球磨机中进行混料并球磨,其中碳催化剂的碳上含有占其重量5%的Pd ; Step a: Preparation of hydrogen absorbing agent, a mass ratio of 3: 1 ratio DEB carbon catalyst powder were mixed and placed in a ball mill for mixing and milling, containing 5% of its weight of Pd on carbon-carbon catalyst;

步骤二:第一层阻氢层的制备,将橡胶胶浆和硫化剂混合并充分搅拌,然后进行低温硫化,最后将硫化后的胶浆倒入模具中,室温下静置,待胶浆表面流动性降低以后将模具放入恒温箱中进行脱水处理,处理后将模具取出,即得到第一层阻氢层; Step two: Preparation of a first layer of a hydrogen barrier layer, the rubber cement was mixed and sufficiently stirred and vulcanizing agent, and then subjected to low temperature curing, after vulcanization dope finally poured into molds and allowed to stand at room temperature until the glue surface after the decrease in flowability the mold was placed in an incubator dehydrated, the processing will remove the mold, to obtain a first layer of a hydrogen barrier layer;

步骤三:分散吸氢剂,将天然橡胶胶浆和硫化剂混合并充分搅拌,然后将步骤一制得的吸氢剂加入到胶浆中,并充分搅拌; Step Three: dispersing hydrogen-absorbing agent, natural rubber and a vulcanizing agent mixed cement and sufficiently stirred, and then the obtained step a hydrogen-absorbing agent is added to the dope, and stirred;

步骤四:第二层吸氢层的制备,将步骤三中得到的胶浆置于30-70°C的水浴中保温30-60分钟,然后将胶浆倒入盛有第一层阻氢层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入恒温箱中,恒温箱温度低于硫化时的水浴温度5-10°C,经过10-30分钟后将模具取出,即得到阻氢层和吸氢层的复合层;步骤五:第三层阻氢层的制备,将橡胶胶浆和硫化剂混合并充分搅拌,然后进行低温硫化,最后将硫化后的胶浆倒入步骤四得到的复合层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入恒温箱中脱水处理,处理后将模具取出,即得到夹层为吸氢层,外层为阻氢层的复合层。 Step Four: Preparation of hydrogen-absorbing layer of the second layer, the dope obtained in step three is placed in a water bath of 30-70 ° C incubation for 30-60 minutes, then poured into a mortar hydrogen barrier layer a first layer molds, allowed to stand at room temperature, the surface will reduce the flowability of cement to be placed in the mold in the oven, the oven temperature is 5-10 ° C lower than the temperature of the water bath when the vulcanization mold after 10 to 30 minutes after removed , i.e. to obtain a hydrogen-barrier layer and the absorbing layer, the composite layer; step five: preparation of a hydrogen barrier layer is a third layer, the vulcanizing agent and rubber cement mixed and sufficiently stirred, and then subjected to low temperature curing, after curing and finally the dope was poured into the mold of the composite layer obtained in step four, allowed to stand at room temperature, the surface will reduce the flowability of cement to be placed in the mold in the oven dehydration treatment process after the mold removed, i.e. to obtain a hydrogen absorbing layer as the interlayer, an outer a hydrogen barrier layer is a layer of a composite layer.

[0005] 在上述技术方案中,步骤二和步骤五中所述低温硫化的硫化温度小于70°C,所述恒温箱内温度要低于硫化温度5-10°C,并经过10-30分钟后将模具从恒温箱内取出。 [0005] In the above aspect, the curing temperature of the fifth step of the low temperature vulcanization step two and less than 70 ° C, the temperature inside the thermostat is lower than the vulcanization temperature 5-10 ° C, and after 10-30 minutes after the mold was removed from the incubator.

[0006] 在上述技术方案中, 所述步骤三中的天然橡胶胶浆和硫化剂的质量比在100:1-200:1之间,且吸氢剂占总质量的3%-8%。 [0006] In the above aspect, the quality of natural rubber cement and curing agent in the ratio of three in step 100: 1-200: 1, and 3% -8% of the total mass of the hydrogen getter.

[0007] 本发明的吸氢层中分散有有机吸氢剂DEB (即:1,4-双(苯基乙炔基)苯),具有最好的吸氢性能,且具有反应速率快和不可逆的特征,当然也可以是其它类型的吸氢材料,并且根据所选择的吸氢材料的不同采用相应的硫化剂和硫化温度。 Absorbing layer [0007] of the present invention are dispersed in an organic absorbing agent, the DEB (i.e.: 1,4-bis (phenylethynyl) benzene), has the best hydrogen storage properties, and has a fast reaction rate and irreversible wherein, of course also be other types of hydrogen-absorbing material, and using the corresponding vulcanizing agent and the vulcanization temperature depending on the selected hydrogen-absorbing material. 阻氢层材料可以采用丁基橡胶或硅橡胶等,可根据不同的橡胶种类选择相应的硫化工艺,但硫化温度要低于中间层即吸氢层天然橡胶的硫化温度,以防止天然橡胶过硫化。 A hydrogen barrier layer material can be used butyl rubber or silicone rubber, may be selected depending on the appropriate vulcanization process of rubber types, but lower than the vulcanization temperature of the intermediate layer i.e. the curing temperature of the hydrogen-absorbing layer, a natural rubber, a natural rubber to prevent overcure . 各层胶浆倒入模具后一定要在室温下静置一段时间,待表面流动性降低后一定要在温度稍低于硫化温度的恒温箱或恒温室中恒温进行脱水处理,以避免温度过高致使过硫化现象的发生。 The layers were poured into a mold dope after a period of time must be allowed to stand at room temperature until the rear surface of the flow must be lowered slightly lower than the vulcanization temperature of the thermostatic chamber or incubator temperature dehydrated at temperatures to avoid overheating resulting in over-curing phenomenon. 在本发明中,与手套箱内气氛直接接触的一层,即外层阻氢层选择氢气阻隔性能尽量优良的橡胶材料,与手套佩戴者直接接触的一层,即内层阻氢层可以选择与人的皮肤相容性好的橡胶材料,以提高佩戴的舒适程度,而对阻氢性能要求可以降低。 In the present invention, a layer in direct contact with the atmosphere in a glove box, i.e., the outer barrier layer have chosen to keep the hydrogen superior hydrogen barrier properties of a rubber material, a layer of the glove in direct contact with the wearer, i.e. the inner barrier layer can be selected hydrogen compatibility with human skin good rubber material to improve the comfort of wear, while the hydrogen permeation resistance requirements can be reduced.

[0008] 从上述本发明的各项技术特征可以看出,其优点是:本发明是通过夹层中的吸氢剂在催化剂的作用下与渗透到手套内的氚发生化学反应,从而将氚以化合物的形式永远留在了手套内,这样不仅起到了保护操作者的作用,同时也起到了降低环境污染和氚回收的作用;本发明的中间吸氢层选用气密性较差的天然橡胶,这样通过外层阻氢层渗透过来的氚在夹层内的迁移速度比在外层气密性较好的橡胶中更快,这样可以提高氚与吸氢剂接触的概率,从而可以提高防止氚向外渗透的效果。 [0008] As can be seen from the technical features of the present invention, its advantages are: the present invention is by dissection permeate hydrogen getter hand jacket tritium in the catalyst chemical reaction, thereby to tritium form of the compound will always remain in the glove, so that not only played a role in the protection of the operator, and also to reduce environmental pollution and plays a role in recovering tritium; intermediate absorbing layer of the present invention is the choice of natural rubber is poor airtightness, such permeation of hydrogen over the barrier layer by layer in the dissection tritium migration rate than the probability of the outer layer rubber is preferably airtight faster, this can increase the hydrogen getter in contact with tritium, tritium can be prevented to improve the outward penetration effect.

附图说明 BRIEF DESCRIPTION

[0009] 本发明将通过附图比较以及结合实例的方式说明: [0009] The present invention will be incorporated by reference and comparison examples illustrate:

图I是本发明三层复合薄膜的吸氢测试结果; Figure I is a hydrogen-absorbing test results of the three-layer composite film according to the present invention;

图2是本发明三层复合薄膜的透氢测试结果。 FIG 2 is a three-layer test results hydrogen permeable composite film of the present invention.

具体实施方式 Detailed ways

[0010] 下面结合附图通过实施例对本发明做进一步的说明。 [0010] DRAWINGS Examples further illustrate the present invention in combination.

[0011] 实施例I [0011] Example I

步骤一:制备吸氢剂。 Step a: Preparation of hydrogen absorbing agent. 按照DEB和碳催化剂(碳上含有占其重量5%的Pd)粉末质量比3 :1的比例配制吸氢剂,放入球磨机中进行混料并球磨I小时。 According DEB and carbon catalyst (containing 5% of its carbon by weight Pd) powder mass ratio of 3: 1 ratio of hydrogen getter formulation, a ball mill and milling for compounding I hour.

[0012] 步骤二:第一层薄膜的制备。 Two [0012] the steps of: preparing a first film layer. 将天然橡胶胶浆和硫化剂按150 :1的质量比混合并充分搅拌,此处的硫化剂可以是硫磺粉、氧化锌等,然后将容器置于50°C水浴中保温50分钟,最后将胶浆倒入模具中,室温下静置,待胶浆表面流动性降低以后将模具放入45°C恒温箱中,约20分钟后将模具取出,即得到第一层薄膜。 Natural rubber cement and curing agent for 150: 1 and thoroughly stirred mass ratio of the vulcanizing agent herein may be sulfur powder, zinc oxide, and then placing the container in 50 ° C water bath and incubated for 50 minutes and finally dope poured into a mold and allowed to stand at room temperature, after the surface of the flow of dope to be lowered into the mold 45 ° C incubator, remove the mold after about 20 minutes, to obtain a first layer of the film. [0013] 步骤三:分散吸氢剂。 [0013] Step Three: dispersing hydrogen getter. 将天然橡胶胶浆和硫化剂按照150 :1的质量比例混合并充分搅拌,然后将步骤一制得的吸氢剂和胶浆混合,并充分搅拌,吸氢剂占总质量的4%。 Natural rubber cement and curing agent for 150: 1 and stirred thoroughly mixing mass ratio, then the step a hydrogen-absorbing agent obtained dope and mixed, and sufficiently stirred, and 4% of the total mass of the hydrogen getter.

[0014] 步骤四:吸氢层的制备。 [0014] Step Four: manufacturing a hydrogen absorbing layer. 将步骤三中得到的胶浆置于50°C的水浴中保温50分钟,然后将胶浆倒入盛有第一层薄膜的模具中,室温下静置,待胶浆表面流动性降低后将模具放入45°C恒温箱中,约20分钟后将模具取出,即得到两层结构的复合薄膜。 The incubation step three dope obtained was placed in a water bath at 50 ° C for 50 minutes, then poured into a mold dope the first layer of thin film and allowed to stand at room temperature, of the surface of the flow will be reduced dope the mold was placed in a 45 ° C incubator, remove the mold after about 20 minutes, to obtain a composite film of two-layer structure.

[0015] 步骤五:第三层薄膜的制备。 Five [0015] Step: Preparation of films of the third layer. 按照步骤二同样制备胶浆并硫化,然后将胶浆倒入步骤四得到的复合层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入45°C恒温箱中,约20分钟后将模具取出,即得到夹层为吸氢层的三层复合薄膜。 Similarly prepared following the procedure two dope and vulcanized, and then the dope was poured into the mold of the composite layer obtained in step four, standing at room temperature, the surface will reduce the flowability of cement to be placed in the mold 45 ° C incubator, after about 20 minutes the mold removed, to obtain a three-layer sandwich composite film of the hydrogen-absorbing layer.

[0016] 实施例2 [0016] Example 2

步骤一:制备吸氢剂。 Step a: Preparation of hydrogen absorbing agent. 按照DEB和碳催化剂(碳上含有占其重量5%的Pd)粉末质量比3 :1的比例配制吸氢剂,放入球磨机中进行混料并球磨I小时。 According DEB and carbon catalyst (containing 5% of its carbon by weight Pd) powder mass ratio of 3: 1 ratio of hydrogen getter formulation, a ball mill and milling for compounding I hour. [0017] 步骤二:第一层薄膜的制备。 Two [0017] the steps of: preparing a first film layer. 将天然橡胶胶浆和硫化剂按100 :1的质量比混合并充分搅拌,此处的硫化剂可以是硫磺粉、氧化锌等,然后将容器置于65°C水浴中保温45分钟,最后将胶浆倒入模具中,室温下静置,待胶浆表面流动性降低以后将模具放入60°C恒温箱中,约15分钟后将模具取出,即得到第一层薄膜。 Natural rubber cement and a vulcanizing agent per 100: 1 and thoroughly stirred mass ratio of the vulcanizing agent herein may be sulfur powder, zinc oxide, and then placing the container in 65 ° C water bath and incubated for 45 minutes and finally dope poured into a mold and allowed to stand at room temperature, after the surface of the flow of dope to be lowered into the mold 60 ° C incubator, remove the mold after about 15 minutes, to obtain a first layer of the film.

[0018] 步骤三:分散吸氢剂。 [0018] Step Three: dispersing hydrogen getter. 将天然橡胶胶浆和硫化剂按照100 :1的质量比例混合并充分搅拌,然后将步骤一制得的吸氢剂和胶浆混合,并充分搅拌,吸氢剂占总质量的3%。 Cement and natural rubber vulcanizing agent according to 100: 1 and stirred thoroughly mixing mass ratio, then the step a hydrogen-absorbing agent obtained dope and mixed, and sufficiently stirred for 3% of the total mass of the hydrogen getter.

[0019] 步骤四:吸氢层的制备。 [0019] Step Four: manufacturing a hydrogen absorbing layer. 将步骤三中得到的胶浆置于70°C的水浴中保温30分钟,然后将胶浆倒入盛有第一层薄膜的模具中,室温下静置,待胶浆表面流动性降低后将模具放入60°C恒温箱中,约15分钟后将模具取出,即得到两层结构的复合薄膜。 The cement was placed in a water bath at 70 ° C obtained in Step Three incubated for 30 minutes and then poured into a mold dope the first layer of thin film and allowed to stand at room temperature, of the surface of the flow will be reduced dope the mold was placed in a 60 ° C incubator, remove the mold after about 15 minutes, to obtain a composite film of two-layer structure.

[0020] 步骤五:第三层薄膜的制备。 The third layer is a thin film preparation: [0020] Step V. 按照步骤二同样制备胶浆并硫化,然后将胶浆倒入步骤四得到的复合层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入60°C恒温箱中,约15分钟后将模具取出,即得到夹层为吸氢层的三层复合薄膜。 Similarly prepared following the procedure two dope and vulcanized, and then the dope was poured into the mold of the composite layer obtained in step four, standing at room temperature, the surface will reduce the flowability of cement to be placed in the mold 60 ° C incubator, after about 15 minutes the mold removed, to obtain a three-layer sandwich composite film of the hydrogen-absorbing layer.

[0021] 实施例3 [0021] Example 3

步骤一:制备吸氢剂。 Step a: Preparation of hydrogen absorbing agent. 按照DEB和碳催化剂(碳上含有占其重量5%的Pd)粉末质量比3 :1的比例配制吸氢剂,放入球磨机中进行混料并球磨I小时。 According DEB and carbon catalyst (containing 5% of its carbon by weight Pd) powder mass ratio of 3: 1 ratio of hydrogen getter formulation, a ball mill and milling for compounding I hour.

[0022] 步骤二:第一层薄膜的制备。 Two [0022] the steps of: preparing a first film layer. 将天然橡胶胶浆和硫化剂按200 :1的质量比混合并充分搅拌,此处的硫化剂可以是硫磺粉、氧化锌等,然后将容器置于45°C水浴中保温55分钟,最后将胶浆倒入模具中,室温下静置,待胶浆表面流动性降低以后将模具放入40°C恒温箱中,约30分钟后将模具取出,即得到第一层薄膜。 Natural rubber cement and a curing agent of 200: 1 and thoroughly stirred mass ratio of the vulcanizing agent herein may be sulfur powder, zinc oxide, and then placing the container in 45 ° C water bath and incubated 55 minutes, and finally dope poured into a mold and allowed to stand at room temperature, after the surface of the flow of dope to be lowered into the mold 40 ° C incubator, remove the mold after about 30 minutes, to obtain a first layer of the film.

[0023] 步骤三:分散吸氢剂。 [0023] Step Three: dispersing hydrogen getter. 将天然橡胶胶浆和硫化剂按照200 :1的质量比例混合并充分搅拌,然后将步骤一制得的吸氢剂和胶浆混合,并充分搅拌,吸氢剂占总质量的8%。 Cement and natural rubber vulcanizing agent according to 200: 1 and stirred thoroughly mixing mass ratio, then the step a hydrogen-absorbing agent obtained dope and mixed, and sufficiently stirred and 8% of the total mass of the hydrogen getter.

[0024] 步骤四:吸氢层的制备。 [0024] Step Four: manufacturing a hydrogen absorbing layer. 将步骤三中得到的胶浆置于40°C的水浴中保温60分钟,然后将胶浆倒入盛有第一层薄膜的模具中,室温下静置,待胶浆表面流动性降低后将模具放入40°C恒温箱中,约30分钟后将模具取出,即得到两层结构的复合薄膜。 The dope obtained in three steps of 40 ° C was placed in a water bath for 60 minutes and then poured into a mold dope layer of the first thin film and allowed to stand at room temperature, of the surface of the flow will be reduced dope the mold was placed in a 40 ° C incubator, remove the mold after about 30 minutes, to obtain a composite film of two-layer structure.

[0025] 步骤五:第三层薄膜的制备。 Five [0025] Step: Preparation of films of the third layer. 按照步骤二同样制备胶浆并硫化,然后将胶浆倒入步骤四得到的复合层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入40°C恒温箱中,约30分钟后将模具取出,即得到夹层为吸氢层的三层复合薄膜。 Similarly prepared following the procedure two dope and vulcanized, and then the dope was poured into the mold of the composite layer obtained in step four, standing at room temperature, the surface will reduce the flowability of cement to be placed in the mold 40 ° C incubator, after about 30 minutes the mold removed, to obtain a three-layer sandwich composite film of the hydrogen-absorbing layer.

[0026] 对上述三个实施例所制作出的三层复合薄膜进行测试,得到如附图I和2所示的结果,其中附图I为制备的三层复合薄膜的吸氢测试结果,纵坐标为DEB的吸氢量与理论吸氢量的比值随时间的变化关系;附图I表明了在天然乳胶硫化后吸氢剂仍具备吸氢能力。 [0026] The above-described three embodiments of the tested embodiment of the created three-layer composite film, to give the results shown in figures I and 2, where I is the reference test result absorbing layer composite films prepared longitudinal coordinates of the ratio of change with time of DEB theoretical hydrogen uptake of hydrogen uptake; Figure I shows the natural latex after vulcanizing agents still have the hydrogen absorbing hydrogen-absorbing capacity. 附图2为三层复合薄膜的透氢测试结果(压差法,测试是在特殊气体透过性测试仪上进行),高压侧采用一个大气压的纯氢,附图2中纵坐标为检测池(真空侧)内氢气压力随时间的变化率。 The test results of hydrogen permeable Figure 2 is a three-layer composite film (differential pressure method, the test is carried out on the tester through a special gas), a high pressure side using the pure hydrogen atmosphere, 2 of the drawings ordinate detection cell the (vacuum side) hydrogen pressure rate of change over time. 图中A曲线为中间夹层中未添加吸氢剂的薄膜的透氢测试结果,图中B曲线为中间夹层中添加了吸氢剂的薄膜的透氢测试结果,对比曲线A和B可以看出,在纯氢测试条件下由于三层复合薄膜中间层内吸氢剂的吸氢作用而使薄膜中的氢达到稳态渗透的时间延长了I小时左右。 A graph in FIG hydrogen permeable intermediate interlayer test result was not added hydrogen getter film, curve B in FIG added Interlayer film hydrogen getter hydrogen permeable test results, comparison of curves A and B can be seen under pure hydrogen absorbing effect of the test conditions because the intermediate layer of a three-layer laminated film of the thin film hydrogen getter reach a steady state permeation of hydrogen prolonged for about I hour. 从而表明中间层添加了吸氢剂的三层复合薄膜具有很好的“阻氢”性能,也即“防止氢渗透”性能。 Indicating that the intermediate layer is added a three-layer composite film having excellent hydrogen-absorbing agent "hydrogen barrier" properties, i.e., "preventing hydrogen permeation" performance. 在手套箱内进行氚操作的过程中,由于氚的浓度非常低,故氚的总量极低,分散在防氚手套内的吸氢剂足以将渗透到手套内的氚吸收掉,从而起到对操作者保护和环境保护的功能。 Tritium during operation in a glove box, since the concentration of tritium is very low, so that the total amount of tritium is very low, dispersion in the glove tritium hydrogen getter sufficient to tritium permeation hand jacket absorbed, and thus play function operator protection and environmental protection.

[0027] 本说明书中公开的所有特征,除了互相排斥的特征以外,均可以以任何方式组合。 All of the features [0027] disclosed in the present specification, except the mutually exclusive features, can be combined in any manner.

[0028] 本说明书(包括任何附加权利要求、摘要和附图)中公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换。 [0028] in this specification (including any accompanying claims, abstract and drawings) disclosed in any of the features, unless specifically described, can be replaced by other equivalent or alternative features having similar purpose. 即,除非特别叙述,每个特征只是一系列等效或类似特征中的一个例子而已。 That is, unless specifically described, each feature is only one example of a series of equivalent or similar features only.

Claims (3)

1. 一种防氚手套的制备方法,其特征在于制作具有三层结构的防氚手套,即第一层阻氢层、第二层吸氢层和第三层阻氢层,具体步骤包括: 步骤一:制备吸氢剂,按照质量比3:1的比例将DEB和碳催化剂粉末混合,放入球磨机中进行混料并球磨,其中碳催化剂的碳上含有占其重量5%的Pd ; 步骤二:第一层阻氢层的制备,将橡胶胶浆和硫化剂混合并充分搅拌,然后进行低温硫化,最后将硫化后的胶浆倒入模具中,室温下静置,待胶浆表面流动性降低以后将模具放入恒温箱中进行脱水处理,处理后将模具取出,即得到第一层阻氢层; 步骤三:分散吸氢剂,将天然橡胶胶浆和硫化剂混合并充分搅拌,然后将步骤一制得的吸氢剂加入到胶浆中,并充分搅拌; 步骤四:第二层吸氢层的制备,将步骤三中得到的胶浆置于30-70°C的水浴中保温30-60分钟,然后将胶浆倒 A method of preparing tritium gloves, comprising fabricating a three-layer structure tritium glove, i.e., a first layer of a hydrogen barrier layer, second layer and third layers absorbing the hydrogen barrier layer, the specific steps include: step a: preparation of hydrogen absorbing agent, a mass ratio of 3: 1 ratio DEB carbon catalyst powder were mixed and placed in a ball mill for mixing and milling, containing 5% of its weight of Pd on carbon-carbon catalyst; step II: preparation of the first layer of the hydrogen barrier layer, the rubber cement was mixed and sufficiently stirred and vulcanizing agent, and then subjected to low temperature curing, after vulcanization dope finally poured into molds and allowed to stand at room temperature until the surface of the flow dope after the mold is lowered into dehydrated incubator, remove the mold after processing, to obtain a first layer of a hydrogen barrier layer; step three: dispersing hydrogen-absorbing agent, natural rubber cement mixed and sufficiently stirred and vulcanizing agent, then a step to prepare hydrogen-absorbing agent is added to the dope, and stirred; step IV: preparation of hydrogen-absorbing layer of the second layer, the dope obtained in step three is placed in a water bath of 30-70 ° C heat for 30-60 minutes, then pour glue 入盛有第一层阻氢层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入恒温箱中,恒温箱温度低于硫化时的水浴温度5-10°C,经过10-30分钟后将模具取出,即得到阻氢层和吸氢层的复合层; 步骤五:第三层阻氢层的制备,将橡胶胶浆和硫化剂混合并充分搅拌,然后进行低温硫化,最后将硫化后的胶浆倒入步骤四得到的复合层的模具中,室温下静置,待胶浆表面流动性降低后将模具放入恒温箱中脱水处理,处理后将模具取出,即得到夹层为吸氢层,外层为阻氢层的复合层。 Into a mold filled with the hydrogen barrier layer of the first layer, allowed to stand at room temperature, the surface will reduce the flowability of cement to be placed in the mold in the oven, the oven temperature is lower than the bath temperature at vulcanization 5-10 ° C, after 10-30 minutes the mold after extraction, i.e. to obtain a hydrogen-barrier layer and the composite layer absorbing layer; step five: preparation of a hydrogen barrier layer is a third layer, the vulcanizing agent and rubber cement mixed and sufficiently stirred, followed by low temperature sulfide, and finally the mold is a composite layer after the curing mortar obtained was poured step four, standing at room temperature, the surface will reduce the flowability of cement to be placed in the mold in the oven dehydration treatment process after the mold removed, i.e., a laminated layer of hydrogen storage, the hydrogen barrier layer, the outer layer is a composite layer.
2.根据权利要求I所述的一种防氚手套的制备方法,其特征在于步骤二和步骤五中所述低温硫化的硫化温度小于70°C,所述恒温箱内温度要低于硫化温度5-10°C,并经过10-30分钟后将模具从恒温箱内取出。 The method for preparing a tritium I according to claim gloves, wherein the curing temperature of the fifth step of the low temperature vulcanization step two and less than 70 ° C, the temperature inside the thermostat is lower than the vulcanization temperature 5-10 ° C, and after 10 to 30 minutes after the mold was removed from the incubator.
3.根据权利要求I所述的一种防氚手套的制备方法,其特征在于所述步骤三中的天然橡胶胶浆和硫化剂的质量比在100:1-200:1之间,且吸氢剂占总质量的3%-8%。 The method of preparing an anti-I tritium glove according to claim, characterized in that the mass of the natural rubber cement and three step curing agent ratio 100: 1-200: 1, and the suction 3% -8% of the total mass of the hydrogen generating agent.
CN 201210420970 2012-10-30 2012-10-30 Method for producing tritium-proof gloves CN102922538B (en)

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