A method for preparing a zero heavy metal salt perfluoroisobutylene protective material

Abstract

The present application relates to the field of protective materials, and particularly relates to a preparation method of zero heavy metal salt perfluoroisobutene protective material; the method comprises the following steps: (a) surface modification of activated carbon: the activated carbon is placed in a tube furnace and heat treated under a nitrogen atmosphere to obtain a surface modified activated carbon carrier; (b) preparation of a non-metal chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane impregnant; (c) loading of the non-metal chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane: the surface modified activated carbon carrier is impregnated in the impregnant, and after drying, an impregnated carbon adsorbent is obtained; the perfluoroisobutene protective material prepared by the preparation method can realize efficient adsorption of perfluoroisobutene. The preparation method is simple in process and convenient in operation, does not use heavy metal salts, is suitable for industrial scale production, is stable in performance, environmentally friendly, and has great industrial economic value.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of protective materials, in particular to a preparation method of zero heavy metal salt perfluoroisobutylene protective material. BACKGROUND

[0002] Perfluoroisobutylene (perfluoroisobutylene) has high toxicity and volatility, and its toxicity is about ten times that of phosgene. Under high humidity conditions, it can easily penetrate the gas mask and is considered as a highly threatening potential chemical warfare agent. It is a by-product of the organic fluorine industry, which is abundant in source and can be used as an emergency toxic agent, so it has received extensive attention from the chemical defense field. The Chemical Weapons Convention (CWC) is one of the strictly controlled chemical hazards, and is also included in our toxic agent protection spectrum as an emergency toxic agent. Therefore, the protection and elimination of PFlB has always been an important topic in the field of chemical defense research.

[0003] The DRES of Canada was the first to start the research and development of PPC, and established a complete set of carbon material research and production facilities for PPC. The United Kingdom has always paid great attention to the protection of perfluoroisobutylene. The Boston Chemical Protection Institute first conducted a detailed study on the ability of ASC impregnated carbon to protect perfluoroisobutylene, and later carried out a long-life impregnated carbon research and development plan with the DERS of Canada, aiming to provide “balanced protection” for all toxic agents including perfluoroisobutylene. At present, the impregnated carbon adsorbent has strong adsorption capacity for single component, single type toxic gas or multiple components and multiple toxic gases. Perfluoroisobutylene, as a representative of toxic agents, can easily penetrate the impregnated activated carbon layer, and perfluoroisobutylene is called a penetrating toxic agent. China has also done a lot of research on the protection of perfluoroisobutylene. The currently produced perfluoroisobutylene protective material has the problems of complex process, high cost, serious environmental pollution and low adsorption capacity. SUMMARY

[0004] The present application provides a preparation method of zero heavy metal salt perfluoroisobutylene protective material to solve the technical problem that ordinary impregnated activated carbon cannot meet the protection requirements of perfluoroisobutylene. The perfluoroisobutylene protective material prepared by the preparation method can realize high-efficiency adsorption of perfluoroisobutylene. The preparation method is simple in process and convenient to operate, does not use heavy metal salt, is suitable for industrialized scale production, has stable performance, high adsorption capacity, relatively low cost and environmental friendliness, and can solve the above technical problems.

[0005] To solve the above technical problems, the technical scheme adopted by the present application is as follows: a preparation method of zero heavy metal salt perfluoroisobutylene protective material, comprising the following steps:

[0006] (a) Surface modification of activated carbon: The activated carbon is placed in a tube furnace, the furnace is filled with nitrogen, and then the temperature is programmed to rise. When the temperature is stable at the target temperature, it is kept constant for a period of time, then cooled to room temperature, and then discharged. The surface-modified activated carbon carrier is obtained;

[0007] (b) Preparation of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane impregnant: Non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane are added to the modified activated carbon and an equal volume of solvent to dissolve, obtaining an impregnant containing non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane;

[0008] (c) Loading of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane: The surface-modified activated carbon carrier is immersed in the impregnant of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane, and after drying, the impregnated carbon adsorbent is obtained.

[0009] Further, the temperature rising rate in step (a) is 5℃ / min, and the heat treatment is carried out at 400-900℃ for 1-4 hours.

[0010] Further, the activated carbon in step (a) includes one of coconut shell carbon, spherical activated carbon and coal-based activated carbon.

[0011] Preferably, the heat treatment refers to heat treatment at 600-800℃ for 2-3 hours in a nitrogen atmosphere.

[0012] Further, in step (b), the non-metallic chloride is ammonium chloride.

[0013] Further, in step (b), the mass proportion of the non-metallic chloride loaded is 0.1-25 wt% of the mass of the modified activated carbon.

[0014] Further, in step (b), the mass proportion of 1,3-bis ((trihydroxymethyl) methylamino) propane loaded is 0.1-10 wt% of the mass of the modified activated carbon.

[0015] Preferably, the mass proportion of 1,3-bis ((trihydroxymethyl) methylamino) propane loaded is 3-8 wt% of the mass of the modified activated carbon.

[0016] Further, in step (b), the drying equipment in step (c) should be an electric heating type air drying machine; the drying temperature is 45-80℃.

[0017] Compared with the prior art, the present application has the following beneficial effects:

[0018] The prepared perfluoroisobutylene protective material can realize high-efficiency adsorption of perfluoroisobutylene.

[0019] Compared with the existing perfluoroisobutylene impregnated carbon adsorbent, the perfluoroisobutylene impregnated carbon adsorbent provided by the application does not add heavy metal salt components, is more economical and environmentally friendly.

[0020] The prepared high-efficiency protective perfluoroisobutylene impregnated carbon adsorbent can realize high-capacity adsorption of perfluoroisobutylene protection, increase the odor gas purification capacity of activated carbon in a complex background atmosphere, realize high-efficiency selective adsorption of perfluoroisobutylene on the basis of the wide-spectrum adsorption performance of impregnated activated carbon, and meet the wide-spectrum purification demand of toxic gases in a complex environment. DETAILED DESCRIPTION

[0021] The application will be further described below in combination with specific embodiments. Embodiment 1

[0022] The embodiment provides a preparation method of high-efficiency protective perfluoroisobutylene impregnated carbon adsorbent, which comprises the following steps.

[0023] (a) Preparation of surface-modified activated carbon: 100 g of activated carbon is placed in a tubular furnace, nitrogen is introduced into the furnace body at a flow rate of 5 L / min, and after the nitrogen is filled, the nitrogen flow rate is lowered to 0.5 L / min. Start the programmed temperature rise at a rate of 5 ℃ / min. After the temperature is stabilized at 800 ℃, keep the temperature constant for 3 hours. After 3 hours, wait for the tubular furnace to cool naturally to room temperature, and then discharge; turn off the nitrogen. The surface-modified activated carbon carrier is obtained.

[0024] (b) Preparation of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane impregnant:

[0025] 18 wt% of ammonium chloride and 8 wt% of 1,3-bis ((trihydroxymethyl) methylamino) propane of the mass of the modified activated carbon are added to the modified activated carbon and dissolved in an equal volume of solvent to obtain an impregnant containing ammonium chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane;

[0026] (c) Loading of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane: the surface-modified activated carbon carrier is immersed in the solution of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane, mixed thoroughly, and then placed for 1 hour. The impregnated activated carbon is placed in an electrically heated air drying machine, the heating temperature is set to 60 ℃, and the heating time is set to 2 hours. The high-efficiency protective perfluoroisobutylene impregnated carbon adsorbent is prepared. Example 2

[0027] A preparation method of high-efficiency protective perfluoroisobutene impregnated carbon adsorbent, comprising the following steps:

[0028] (a) Preparation of surface modified activated carbon: 100 g of activated carbon is weighed and placed in a tube furnace, nitrogen is introduced into the furnace body, the nitrogen flow is 5 L / min, after the nitrogen is filled, the nitrogen flow is adjusted to 0.5 L / min. Start the temperature program, the heating rate is 8 ℃ / min. After the temperature is stabilized to 900 ℃, keep the temperature for 3 hours. After 3 hours, wait for the tube furnace to cool down to room temperature, then discharge; turn off the nitrogen. The surface modified activated carbon carrier is obtained.

[0029] (b) Preparation of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane impregnant:

[0030] 15 wt% of ammonium chloride and 5 wt% of 1,3-bis ((trihydroxymethyl) methylamino) propane of the mass of the modified activated carbon are added to the modified activated carbon and dissolved in the same volume of solvent, to obtain an impregnant containing ammonium chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane;

[0031] (c) Loading of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane: the surface modified activated carbon carrier is impregnated in the solution of non-metallic chloride and 1,3-bis ((trihydroxymethyl) methylamino) propane, and after sufficient mixing, it is placed for 1 hour. The impregnated activated carbon is placed in an electric heating type air drying machine, and the heating temperature is set to 55 ℃, and the heating time is 2 hours. The high-efficiency protective perfluoroisobutene impregnated carbon adsorbent is prepared.

[0032] The performance test results of the impregnated carbon are shown in the following table:

[0033]

[0034] Compared with the existing protective material PP carbon, the high-efficiency protective perfluoroisobutene impregnated carbon adsorbent prepared by the preparation method has a longer protective time for perfluoroisobutene and a better effect.

Claims

1. A process for the preparation of a zero heavy metal salt perfluoroisobutylene protective material, characterized by, The method comprises the following steps: (a) surface modification of activated carbon: the activated carbon is placed in a tube furnace, the furnace is filled with nitrogen, and then the temperature is raised at a rate of 5°C / min. The temperature is raised to 400-900°C and the activated carbon is heated for 1-4 hours. After cooling to room temperature, the activated carbon is discharged. The surface-modified activated carbon carrier is obtained; (b) preparation of the impregnant of ammonium chloride and 1,3-bis(trishydroxymethyl)methylamino)propane: ammonium chloride and 1,3-bis(trishydroxymethyl)methylamino)propane are dissolved in an equal volume of solvent to obtain an impregnant containing ammonium chloride and 1,3-bis(trishydroxymethyl)methylamino)propane; (c) loading of ammonium chloride and 1,3-bis(trishydroxymethyl)methylamino)propane: the surface-modified activated carbon carrier is impregnated in the impregnant of ammonium chloride and 1,3-bis(trishydroxymethyl)methylamino)propane, and then dried to obtain an impregnated carbon adsorbent. The mass proportion of ammonium chloride loaded on the modified activated carbon is 0.1-25 wt%, and the mass proportion of 1,3-bis(trishydroxymethyl)methylamino)propane loaded on the modified activated carbon is 0.1-10 wt%.

2. A process for the preparation of a zero heavy metal salt perfluoroisoprene protective material according to claim 1, characterized in that, The activated carbon in step (a) comprises one of coconut shell carbon, spherical activated carbon and coal-based activated carbon.

3. The method for preparing a perfluoroisobutylene protective material with zero heavy metal salts according to claim 1, characterized in that, The drying equipment in step (c) is an electric heating air drying machine, and the drying temperature is 45-80°C.

Images