RU2132226C1 - Method of preparing sorbent for removing water and heavy metals from petroleum derivatives - Google Patents

Abstract

FIELD: petroleum processing. SUBSTANCE: method is distinguished by impregnating fibrous cellulose-containing material with 5 to 15 wt.% of titanium dioxide (active substance), impregnation being performed with 2-5-% solution of titanium tetrachloride in C₅-C₇- hydrocarbons and followed by hydrolysis with water and drying. EFFECT: increased sorption capacity. 1 tbl, 6 ex

Description

 The invention relates to the field of production of new adsorption materials and can be used to purify water from oil products, iron ions, nickel and suspended particles.

 A known method of producing an adsorbent based on titanium with a pore size of 5-40 microns. The filtering method through it provides a residual content of iron ions in water up to 0.19 mg / l [RU, 2006471, MKI 5 C 02 F 1/04, 01 D 39/00, BI N 2, 01/30/94].

 The disadvantages of this method include the significant problem of regeneration of the filter, the high cost and complexity of manufacturing.

A known method of producing an adsorbent by applying salts of FeSO ₄ and FeCl ₃ on the waste products of the production of cotton cellulose composition trap canvas and cyclone dust treated with liquid ammonia. [Pat. USSR N 1731737, MKI 5 C 02 F 1/52, BI 17, 05/05/07].

 The disadvantages of this method include the irrational consumption of iron salts, the frequent replacement of the filling of the filter, due to this the cost of the process.

There is also a method of producing a sorbent for water purification based on vermiculite with a particle size of 0.25-2 mm by treatment with a 30-40% aqueous solution of lignosulfonate at a ratio of 1: 6-24 and heat treatment of the resulting product at 550-700 ^o C. The method allows to increase the adsorption capacity of dissolved petroleum products in comparison with the known method in 1.2-1.7 times. [USSR, 1632946, MKI 5 C 02 F 1/28, cl. D 01 J 20/30, BI N 09, 03/31/07.

 The disadvantages of this sorbent include high energy consumption, high heat treatment temperature, which significantly increases the cost of the product.

Closest to the proposed technical solution is a method for producing a sorbent for purifying solutions of amines, in which titanium dioxide is deposited on a fibrous support — glass fiber — by treatment with titanium tetrachloride vapors, followed by hydrolysis with water and drying. (A.S. USSR N 1650242, B 01 J 20/00, 1991)
However, due to the small capacity of the glass fiber, it is impossible to apply a sufficient amount of titanium oxide, as a result of which the capacity of the resulting sorbent is insufficient.

 The task of the invention is to obtain a high-capacity sorbent for oil, oil products, as well as iron and nickel ions, suitable for household filters.

This task is achieved by modifying the surface of natural cellulosic fibrous materials with titanium dioxide, applied to the surface of the fibers by sorption of TiCl ₄ from an aliphatic solution of C ₅ -C ₇ followed by hydrolysis of H ₂ O and drying. Application of the solute ensures its uniform distribution throughout the volume. The presence of carbonyl groups in the cellulosic material allows you to create a strong bond due to the formation of a hydrogen bond between the carbonyl groups and titanium dioxide, which provides high resistance of the modifier to water leaching. The presence of a modifier can significantly increase the capacity of the adsorbent and provide a wider range of extractable substances, since TiO ₂ is a good adsorbent, and fibrous materials can increase its working surface.

 As natural fibrous materials can be used: cotton wool, gauze, textile waste and other cellulose-containing products.

Example 1. 0.47 g (1.02%) of TiCl _{4 are} dissolved in 70 ml of hexane. The resulting solution is impregnated with 9.8 g of gauze and dried. Then it is washed with water until the washings are neutral, and again dried to constant weight. The mass of the finished adsorbent was 10 g with a content of TiO ₂ = 2%.

Example 2. In 70 ml of hexane was dissolved 1.19 g (2.58%) of TiCl ₄ . The resulting solution is impregnated with 9.5 g of gauze and dried. Then it is washed with water until the washings are neutral, and again dried to constant weight. The mass of the finished adsorbent is 10 g with a content of TiO ₂ = 5%.

Example 3. 2.38 g (5.15%) of TiCl _{4 are} dissolved in 70 ml of hexane. The resulting solution is impregnated with 9 g of gauze and dried. Then it is washed with water until the washings are neutral, and again dried to constant weight. The mass of the finished adsorbent was 10 g with a content of TiO ₂ = 10%.

Example 4. In 70 ml of hexane was dissolved 3.57 g (7.73%) of TiCl ₄ . The resulting solution is impregnated with 8.5 g of gauze and dried. Then it is washed with water until the washings are neutral, and again dried to a constant weight. The mass of the finished adsorbent was 10 g with a content of TiO ₂ = 15%.

Example 5. 2.38 g (5.15%) of TiCl _{4 are} dissolved in 70 ml of hexane. The resulting solution is impregnated with 9 g of medical bleached cotton and dried. Then it is washed with water until the washings are neutral, and again dried to constant weight. The mass of the finished adsorbent was 10 g with a content of TiO ₂ = 10%.

Example 6. 2.38 g (6.01%) of TiCl _{4 are} dissolved in 60 ml of hexane. The resulting solution is impregnated with 9 g of cellulose (GOST 595-79) and dried. Then it is washed with water until the washings are neutral, and again dried to constant weight. The mass of the finished adsorbent was 10 g with a content of TiO ₂ = 10%.

 On the obtained adsorbents, the maximum capacities for oil emulsion, iron and nickel ions were determined.

 The data are given in the table.

 Thus, the proposed method allows to obtain sorbents that purify contaminated water to the necessary environmental standards, this sorbent can be used in both household and technical filters.

Claims (1)

A method of producing a sorbent for water purification from oil products and heavy metals, comprising treating the fibrous carrier with titanium tetrachloride followed by hydrolysis with water and drying, characterized in that cellulose-containing material is used as the fibrous carrier, titanium tetrachloride is used in the form of its 2-7% solution in hydrocarbons C ₅ - C ₇ , the process is carried out to the content of titanium dioxide in the sorbent from 5 to 15 wt.%.

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