JPH01167207A - Method for extracting phosphor from slime - Google Patents

Abstract

PURPOSE: To make it possible to completely extract phosphorus even at the time of treating slime having any degree of stabilization by using surfactants and polyampholytes as org. reagents and treating reagents by heating.

CONSTITUTION: The surfactants (nonionic and anionic active) and/or the polyampholytes are used as the org. reagents according to the compsn. of the slime determined by the characteristics of a stabilizer. The action of the selected org. reagents is based on their emulsion breaking activity. Since these org. reagents have high adsorption activity, the reagents substitute and deflocculate the stabilizer. In the case of the slime stabilized by Ca soap, the surfactant of the anionic activity, like a synthetic resin partly neutralized with alkaline is proposed. The slime is put into a reactor, where the slime is heated to about 70°C and is subjected to an agitation treatment with the org. reagents described above.

COPYRIGHT: (C)1989,JPO

Description

Detailed Description of the Invention Field of the Invention The present invention relates to the production of phosphorus, and more particularly to a method for extracting phosphorus from slime.

The present invention applies to the treatment of slimes produced as a by-product in the production of phosphorus, which are of various compositions and can be stored for various periods of time.

Prior Art Due to the complex structure of slime, there are a variety of prior art methods for extracting phosphorus from slime. Slime is an aqueous emulsion of phosphorus that is stabilized by various emulsifying agents of organic or inorganic origin, such as asphalt-resinous compounds, soot, finely dispersed mineral dust.

The flocculation stability of phosphorus slime is characterized by the dispersibility of phosphorus particles, which depends on the nature of the stabilizer.

To stabilize low stability phosphorus emulsions, low molecular weight hydrocarbons (calcium soaps), so-called "oils" are used. The most stable slimes are stabilized with asphalt-resinous compounds, and the higher the concentration of these compounds in the slime, the more difficult it is to extract phosphorus from the slime.

The type of stabilizer depends first of all on the composition of the raw material to be treated, the extent of its preparation and the technology of phosphorus production.

Since there are various structural elements in the composition of the protective layer of phosphorus particles, it is necessary to use a variety of reagents to destroy these structural elements. Among these reagents are chlorinated hydrocarbons, carbon disulfide, pyrolytic resins, hexavalent chromium compounds in acidic media, hydrogen peroxide in phosphoric acid.

The use of non-renewable critical inorganic reagents in the process of extracting phosphorus from slime makes the process uneconomical and pollutes the environment with toxic substances.

Methods for extracting phosphorus from slime by heating and treating the slime with organochlorine reagents in the presence of hydrogen peroxide are known in the art. The mass ratio of organic reagent to phosphorus in the slime is 8-10:1 (SU, A, 856976).

The extraction of phosphorus from slime guts by this method is based on the extraction of organic stabilizers of phosphorus emulsions with chlorinated hydrocarbons in the presence of oxidizing agents. The key requirement for the extraction of the stabilizers is the use of large amounts of extractant, which complicates the technical process and makes it even more expensive.

Corrosion-resistant equipment must be used because chlorinated hydrocarbons partially hydrolyze resulting in the formation of hydrochloric acid and enhance the corrosive activity of the reaction medium.

This method allows phosphorus extraction with high yields only when processing poorly stabilized phosphorus slimes.

This is determined by the nature of the extractant.

Slime stabilized with asphalt-resinous compounds cannot be treated in this manner.

Solution The main objective of the present invention is the extraction of phosphorus from slime by selecting suitable organic reagents that guarantee complete extraction of phosphorus when processing slime of any degree of stabilization. The purpose is to provide a method.

Means for solving the problem This objective proposes a method of extracting phosphorus from slime by treating the slime with organic reagents during heating,
In this method, this is achieved by using surfactants and/or polyampholytes as organic reagents.

The method proposed here guarantees almost complete extraction of phosphorus from slimes characterized by different degrees of stabilization and storage times. The reagents used do not contaminate phosphorus (and provide favorable conditions for the purification of wastewater from suspensions. These reagents are versatile with respect to various types of slime, are readily available, inexpensive and , and corrosion inert, which greatly simplifies the engineering of the method.

For maximum extraction of phosphorus from slime stabilized with asphalt-resinous compounds, the slime should be
It is advisable to treat with a surfactant such as oxyethylated alkylphenol in an amount of 0.5-10 g per ton.

To extract phosphorus from slime stabilized with calcium soap (“oil”), 0.5-
Preferably, an amount of 10% of partially neutralized fatty acids is used as surfactant.

To extract phosphorus from slime stabilized with molecular colloidal emulsifiers (resins), polyampholytes such as partial hydrolysis products of polyacrylonitrile are used in amounts of 10-100 g per ton of slime. This is desirable.

In order to treat slimes with a phosphorus content of 30-40% by weight and stabilized with organic and inorganic components, a mass ratio of 1:3 (1-100 hydroxyethylated alkylphenols and polyacrylonitrile partial hydrolysis products) is used. It is advisable to use a mixture with

Matakai ■Tachieki The method of the present invention is accomplished in the following manner.

To extract phosphorus from slime, a by-product of phosphorus production, the slime is treated with an organic reagent.

Depending on the composition of the slime, which is determined by the properties of the stabilizer, it is proposed to use surfactants (nonionic and anionically active) and/or polyampholytes as organic reagents.

The action of the organic reagent chosen is based on its demulsifying activity. Since these organic reagents have high adsorption activity,
Displace stabilizer and peptize.

To extract phosphorus from slime stabilized with calcium soaps (low molecular hydrocarbons, "oils"), it has been proposed to use anionically active surfactants, such as synthetic fatty acids partially neutralized with alkali. be done. The action of such demulsifiers is based on a phase inversion that consists in converting insoluble calcium soaps into soluble sodium soaps and removing the film from the phosphorus particles, thereby creating favorable conditions for the coalescence of the particles.

Due to its easy availability, it is expedient to use the bottom residue remaining after the oxidative treatment of paraffins as synthetic fatty acids and to subject the residue to partial neutralization. The demulsifier is introduced into the slime in an amount of 0.5-10% of the weight of the slime. The “armor” contains a predominant content of asphaltenes.
ng)”Solid emulsifier (asphaltene, asphalt-
In order to extract phosphorus from slimes stabilized with resinous compounds), the action is based on the hydrophilization of the hydrophobic surface of the emulsifier and subsequent conversion of the emulsifier into the aqueous phase and additional peptization. It is proposed to use nonionic surfactants that are As a result, the surface of the phosphorus particles is purified and the particles coalesce into large particles. As nonionic surfactant it is proposed to use hydroxyethylated alkylphenols in an amount of 0.5-10 g per ton of slime to be treated. The use of polyampholytes is proposed to extract phosphorus from slime stabilized by molecular colloidal emulsifiers (resins) adsorbed on the phosphorus particle surface for surface activity.

It is recommended to use an amount of polyacrylonitrile partial hydrolysis product as polyampholyte in an amount of 10-100 g per ton of slime.

Polyelectrolytes destroy phosphorus emulsions because they adsorb instead of emulsifiers. Although polyelectrolyte molecules are much more strongly adsorbed to the phosphorus particles than the initial stabilizers of the slime, they are disadvantageous for the formation of stable films and cause coalescence of the particles as they destroy the film. Moreover, the agglomeration of suspended particles by long-chain polyelectrolyte molecules promotes the coalescence of phosphorus particles within the slime.

In order to extract phosphorus from slimes containing large amounts of inorganic impurities (up to 20% by weight) and relatively small amounts of phosphorus (up to 40% by weight), hydroxyethylated alkylphenols and polyphenols in a weight ratio of 1:30-100 are used. The use of mixtures with acrylonitrile partial hydrolysis products is recommended.

The effective destruction of such slimes by the mixture is such that the polyelectrolyte molecules cross-link the inorganic particles and the hydroxyethylated alkylphenol molecules destroy the organic stabilizers and "sheath" emulsifiers, converting the emulsifiers into the aqueous phase. This is due to a clearly significant cooperative effect that makes it possible to do so. This synergistic effect is most pronounced when using the reagents in the above mass ratios.

A special embodiment implementing the method of the invention is shown below for purposes of illustration.

A slime containing 50% phosphorus, 10% solids, and 40% water (by mass %), stabilized primarily with low-molecular hydrocarbons ('oil'), is treated to extract the phosphorus.
g) is placed in a reactor, heated to 70° C., and stirred with 0.5 g of partially neutralized fatty acid (C+ 6Cz + ). Processing time is 1 hour.

After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water. The yield of phosphorus is 90% by weight.

Example 2 A slime containing (by weight %) 60 phosphorus, 5 solids, 35 water is treated to extract the phosphorus, stabilized primarily with low molecular weight hydrocarbons ('oil').

Slime (100 g) is placed in a reactor, heated to 70°C, and stirred with 3 g of partially neutralized fatty acid (C10C21). Processing time is 1 hour. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The phosphorus yield is 99.5%.

Example 3 Stabilized primarily by low molecular weight hydrocarbons (“oils”) and asphalt-resinous compounds (in % by weight)
A slime containing 40 phosphorus, 15 solids, and 45 water is treated to extract phosphorus. Slime (100g) was placed in a reactor, heated to 70°C, and 5g of partially neutralized fatty acids (C
+ b Cz + ). Processing time is 2
It's time.

After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 96% by weight.

Example 4 Predominantly asphalt-stabilized with resinous compounds,
A slime containing (in weight percent) 57 phosphorus, 12 solids, and 31 water is treated to extract the phosphorus.

Slime (100 g) is placed in a reactor, heated to 70° C., and stirred with 5 g of partially neutralized fatty acid (C10C21). Processing time is 2 hours.

After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 90% by weight.

Real-life forceps stabilized primarily with asphalt-resinous compounds,
A slime containing (in weight percent) 65 phosphorus, 5 solids, and 30 water is treated to extract the phosphorus.

The slime (100 g) is placed in a reactor, heated to 70° C. and stirred with 0.05 mg of hydroxyethylated alkylphenol. Processing time is 2 hours. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 98% by weight.

Example 6 Predominantly asphalt-stabilized with resinous compounds,
A slime containing (in % by weight) m 60 , 8 solids, 32 water is treated to extract the phosphorus.

The slime (100 g) is placed in a reactor, heated to 70° C. and stirred with 0.2 mg of hydroxyethylated alkylphenol. Processing time is 2 hours. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The phosphorus yield is 99.5%.

Fact 1 Reference 1 Mainly stabilized with asphalt-resinous compounds,
A slime containing 55% phosphorus, 12% solids, and 33% water is treated to extract the phosphorus.

The slime (100 g) is placed in a reactor, heated to 70° C. and stirred with 1 mg of hydroxyethylated alkylphenol. Processing time is 2 hours. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 95% by weight.

Example 8 A primarily resin-stabilized slime containing (in weight percent) 67 phosphorus, 7 solids, and 26 water is treated to extract the phosphorus. Put the slime (100g) into the reactor and
C. and stirred with 1 mg of polyacrylonitrile partial hydrolysis product. Processing time is 1 hour.

After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The phosphorus yield is 95.5%.

A slime containing (by mass %) 67 phosphorus, 7 solids, and 26 water is treated to extract the phosphorus, primarily stabilized with resin. Put the slime (100g) into the reactor and
C. and stirred with 5 mg of polyacrylonitrile partial hydrolysis product. Processing time is 1 hour.

After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 98% by weight.

Example 10 A primarily resin-stabilized slime containing (in weight percent) 67 phosphorus, 7 solids, and 26 water is treated to extract phosphorus. Put the slime (100g) into the reactor and
℃ and stirred with Log polyacrylonitrile partial hydrolysis product. Processing time is 1 hour. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 99.9% by weight.

fruit ffi 50 phosphorus, 12 solids (in % by weight) stabilized mainly with asphalt-resinous compounds with a predominant content of resins
, the slime containing water 38 is treated to extract phosphorus. Put the slime (100g) into the reactor and
and stirred with 1.0 mg of polyacrylonitrile partial hydrolysis product. Processing time is 2 hours.

After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 95% by weight.

Storm blaze ↓ Phosphorus 40 (in mass %) stabilized primarily with asphalt-resinous compounds with a predominant content of asphaltenes
, 15 solids, and 45 water is treated to extract phosphorus. The slime (100 g) is placed in a reactor, heated to 70° C. and stirred with 6.2 mg of a mixture of hydroxyethylated alkylphenol and polyacrylonitrile partial hydrolysis product in a tt ratio of 1:30. Processing time is 2 hours. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 95.5% by weight.

Performance test ±↓ Phosphorus 45 (in % by weight) stabilized primarily with asphalt-resinous compounds with a predominant content of asphaltenes
, solids 18, and water 37 is treated to extract phosphorus. The slime (100 g) is placed in a reactor, heated to 70° C. and treated with stirring with 10.1 mg of a mixture of hydroxyethylated alkylphenol and polyacrylonitrile partial hydrolysis product in a mass ratio of 1:100. Processing time is 2 hours. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 99% by weight.

Example 14 Phosphorus 38 (in % by weight) stabilized primarily with asphalt-resinous compounds with a predominant content of asphaltenes
, solids 20, and water 42 is treated to extract phosphorus. Slime (100 g) was placed in a reactor, heated to 70 °C and treated with stirring with 5.1 mg of a mixture of hydroxyethylated alkylphenol and polyacrylonitrile partial hydrolysis product in a mass ratio of 1:50. . Processing time is 2 hours. After the slime has separated into a phosphorous layer and an inorganic layer, the latter is flushed out of the reactor with water.

The yield of phosphorus is 97.5% by weight.

The reagent proposed by the present invention ensures maximum extraction of phosphorus from slimes with different degrees of stabilization and storage. The proposed reagent, in addition to its main use as a demulsifier, enters wastewater and is advantageous in purifying wastewater suspensions to flocculate colloidal particles and for its hydrophilization and decomposition. Clean slime deposits from pipes and equipment due to glue action. The method proposed by the present invention does not pollute the environment with toxic substances.

Claims (5)

[Claims] (1) A method for extracting phosphorus from slime by treating the slime with an organic reagent during heating, characterized by using a surfactant and/or a polyampholyte electrolyte as an organic reagent. (2) Process according to claim 1, characterized in that hydroxyethylated alkylphenols are used as surfactant in an amount of 0.5-10 g per ton of slime. (3) A method according to claim 1, characterized in that 0.5-10% of partially neutralized fatty acids are used as surfactants based on the weight of the slime. (4) Use a polyacrylonitrile partial hydrolysis product as a polyampholyte polymer electrolyte, and add the product to slime 1.
Process according to claim 1, characterized in that it is used in an amount of 10-100 g per ton. (5) Claims (1) and (2) characterized in that a mixture of hydroxyethylated alkylphenol and polyacrylonitrile partial hydrolysis product is used in a mass ratio of 1:30-100. The method described in paragraphs and paragraphs (4).