The method of obtaining chemisorptive fiber

 

(57) Abstract:

Usage: in the various fields of the national economy as a fibrous ion exchangers. The inventive source fiber from polyacrylonitrile, a copolymer or polyvinyl chloride is treated with a modifying agent for the circulation and 20 - 90oC. Press to gain a working solution 50-200 wt %. Then heated at 100 - 140oFrom 10 - 120 minutes 3 C.p. f-crystals.

The invention relates to the production of chemisorptive fibers by polymineralic transformations fiber-based chain polymers, in particular on the basis of polyacrylonitrile, copolymers of polyacrylonitrile or polyvinyl chloride.

A method of obtaining an ion-exchange fibers based on polyacrylonitrile processing fiber 50% alcoholic solution of hydrazine hydrate is added at 70oC for 1 6 h, followed by washing with methanol and drying at 60o[1]

According to the method [2] POLYACRYLONITRILE fiber fill a 5% solution of dimethylformamide and treated for 30-60 min at 20oC. Then enter hydrazinehydrate to obtain a solution with a concentration of 75% of the module of the bath 20. The treatment is carried out for 2 hours at 80 100oWith, then netmite fiber, up to 10 is of cation-exchange properties of the fiber is treated with 5 to 20% aqueous solution of alkali at 60 100oFrom 5-60 minutes

These methods are multi-stage, duration of processes a large quantity of the modifying agent. The consumption of reagents is determined by the number of working solutions (typically 250 to 300%) remaining on the surface of the fiber and directed to the regeneration or drains.

The technological process can be performed by treating the freshly-formed PAN-fiber solutions of reagents, followed by additional heating or modifying processing solutions, and the subsequent warm-up or treatment significantly (10 to 100 times) greater than the residence time of the PAN-fibers in baths molding or finishing [3]

Usually getting chemisorptive fibers by chemical transformations of macromolecules carry on the type of equipment that is used for finishing and dyeing, chemical fiber [4] According to a known method [4] fiber loaded into a perforated basket that is placed in the chemical processing apparatus (autoclave), and then processes the circulating solutions of modifying agents, washed and dried. In this arrangement, the process uniformity of the processing depends on the density of the packing of the fibers in the basket of the apparatus and is nedostatek">

The closest technical solution is a method for chemisorption fiber processing of the original PAN-fibers with an aqueous solution of the modifying agent and heated at 100 120oC for 120 minutes and Then the fiber is treated with an aqueous-alkaline solution, washed, squeezed and dried [5]

However, this method has the same disadvantages as the above-described methods, i.e., high consumption of reagents used for regeneration.

The purpose of the invention to create a more efficient process of obtaining chemisorptive fiber, as well as expansion of the range.

This goal is achieved due to the fact that the method of obtaining chemisorptive fiber source fiber-based chain polymer with an aqueous solution of the modifying agent, by heating at an elevated temperature, rinsing, wringing and drying, according to the proposal, the processing is subjected to fiber, loaded into a perforated basket that is placed in a chemical processing apparatus, in the form of cake, press it to the contents of the solution on the fiber 50 to 250%, and the heating is carried out at a flow of coolant in the jacket of the apparatus. Heating is carried out at 100 140oC for 10-120 minutes In the quality of the Yes, and as the modifying agent aqueous solutions of hydrazine hydrate is added, epichlorohydrin and amino compounds at a concentration of 2 to 30 wt. Processing fiber modifying agent can be accomplished by centrifugation, and the continuous flow of reagent solutions at speeds 60-240 rpm

The proposed method allows to reduce the number of agents remaining on the surface of the fibers after chemical modification, i.e. reduced consumption of reagents aimed at regeneration or waste water. In addition, the proposed method allows to extend the range of fibrous ion exchangers, because you can get not only chemisorptive fibers based on polyacrylonitrile and its copolymers, but also on the basis of polyvinyl chloride.

The invention is illustrated by the following examples.

Example 1. 100 g of acrylic fibre loaded into a perforated basket, placed in a chemical processing apparatus, add 100 g of a 25% aqueous solution of hydrazine hydrate is added and heated for 120 min at 100oWith the path of the coolant in the jacket of the apparatus. The concentration of hydrazine hydrate is added (YY) in the wash water after the reaction gidratirovana flow rates of 30 l/kg is 4 centrali 35 g/l, module 1 12, a temperature of 80oC. Receive cation-exchange fiber with SOY on carboxyl groups of 5.7 to 6.0 mEq/g, the strength of 6.5 CN/Tex, an elongation of 35%

Example 2. 10 kg of acrylic fibre loaded into a perforated basket, placed in a chemical processing apparatus and process for the circulation of a 30% aqueous solution of hydrazine hydrate is added at 20oWith module 1 12, within 30 minutes then the solution is drained, the fiber wring out with compressed air content of mortar 150 wt. and heated to 120 min at 120oC. the Concentration of GH in the wash water at a flow rate of wash water 30 l/kg is of 0.44 g/L. After reaction gidratirovana fiber is treated for 30 min with a solution of alkali at a concentration of 35 g/l module 1 to 12 and a temperature of 80oC. Receive cation-exchange fiber with SOY on carboxyl groups of 5.7 to 6.0 mEq/g, the strength of 6.5 CN/Tex, an elongation of 25% YY in the wash water is missing.

Example 3. The fibre is obtained analogously to example 2, but the processing solution YY carried out in a basket centrifuge at 90oC for 10 min and the rotation speed of 240 rpm Then stop circulation, wring out the fiber content of the solution to 500 wt. stop the centrifuge and heat the fiber to 140oWith by podno washed and treated with a solution of sodium hydroxide according to example 1. Get a cation-exchange fiber with the same indicators. Hydrazinehydrate in the wash water is missing.

Example 4. 100 g of fibres based on polyvinyl chloride load in the centrifuge and treated with a 15% solution of ethylene diamine at 20oC for 20 minutes Then stops the circulation of the solution and carry out the processing of the fiber according to example 2 at 120oC for 90 minutes Then the fiber is washed. Receive anion-exchange fiber with SOY 0.1 n HCl 2.5 mg-EQ/g, the Content of ethylene diamine in the wash water at a flow rate of 30 l/kg 0.1 mg/l, which allows the process without regeneration amineralo reagent.

Example 5. 150 g of acrylic fibre loaded into the centrifuge, where it is processed to a 25% aqueous solution BIENNIUM for 90 min at 100oWith module 1 2 and the rotation speed of 60 rpm Then the fiber wring out 10 min before the content of the working solution of the fiber 60% washed with water and treated with an aqueous solution of sodium hydroxide at a concentration of 20 g/l, a temperature of 70oC for 0.5 hours and Then the fiber is squeezed and washed with acidified water. The number of YEARS in the wash water after the stage of gidratirovana reduced in comparison with the prototype in 5 times and is 4 mg/L. Poluchennoy within one party is 0.3 mEq/g

Example 6. 100 g of fiber on the basis of a copolymer of Acrylonitrile (an) with 2-methyl-5-vinylpyridine (IMP) (latest content of 35 wt.) loaded into a perforated basket, placed in a chemical processing apparatus and treated with 30oWith module 1 12 3% aqueous solution of epichlorohydrin (ECG) for 30 min, the solution is drained, the fiber wring out with compressed air content of mortar 100%(wt.) and heated for 60 min at 105oC, washed and dried. Get a strongly basic anion-exchange fiber VION AC-1 with SOY on strong-base groups of 1.0 to 1.2 mEq/g, total capacity (OYe) is 2.4 mEq/year Consumption of epichlorohydrin is 30 g/kg fiber, lavage epichlorhydrin and products of its decomposition are missing.

Example 7 (comparative). 100 g of acrylic fibre is treated with a 25% aqueous solution GG, after which it is heated at 120oC for 120 min, and then amyraut 10% aqueous solution of sodium hydroxide for 30 min at 95 98oWith module and bath 50. The concentration of GH in the wash water at a flow rate of wash water 33 l/kg 20 g/L. After alkaline hydrolysis get a cation-exchange fibers with the same physical and mechanical properties and SOYBEANS, as in the proposed method.

2. The method according to p. 1, wherein the heating is carried out at 100-140C for 10-120 minutes

3. The method according to p. 1, characterized in that the treatment machine based fiber polyacrylonitrile, Acrylonitrile copolymers, or polyvinyl chloride.

4. The method according to p. 1, characterized in that the modifying agent used aqueous solutions of hydrazine hydrate is added, epichlorohydrin or amino compounds at a concentration of 2-30 wt.

 

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2 ex

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Abstract // 2293061

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