Composite moisture-retaining material and method of obtaining thereof

FIELD: chemistry.

SUBSTANCE: invention relates to a composite moisture-retaining material, which can be used in crop production for the improvement of water-air and nutritional mode of soil, as well as for the recovery of vegetation on soils of various types. The composite moisture-retaining material is made on the base of acryl copolymer and filler. The acryl copolymer is made on the base of acrylamide and acrylic acid salts with a ratio of 20/80-80/20 mol. % in the presence of a cross-linking agent N,N'-methylene-bis-acrylamide and a polymerisation initiator. As the filler used is a mixture of wastes of biocatalytic productions of acryl monomers and acids of humic acids with a ratio of 99/70-1/30 wt % by dry substance in the form of a water paste or a dry powder-like form. The total content of the filler constitutes to 60 wt %. A method of obtaining the composite moisture-retaining material is described.

EFFECT: reduced cost of the moisture-retaining material, presence of an additional source of plant nutrition, simplification of technology of a filled gel manufacturing with the preservation of water-sorption properties at the level of existing filled and non-filled analogues.

2 cl, 1 tbl, 10 ex

 

The invention relates to agriculture and can be used in plant breeding to improve water, air and nutrient regime of the soil, and restoration of vegetation on soils of different types.

Currently, in regions with low climatic moisture soil applied polymer materials having a high degree of water absorption (up to several hundreds of grams of water per 1 g initial dry polymer). Their use allows for a more stable plants to tolerate periods of abrupt climate changes, to reduce water consumption for irrigation in 1,5-2 times, reduce leaching of soils, fertilizers and micronutrients. The most effective are acrylic polymeric materials with three-dimensional mesh structure, and the use of different combinations of monomers makes it possible to form a copolymer with the desired consumer and operational properties for different soil types.

In Russia the wide application of these materials in agriculture for planting urban and industrial landscapes prevents their high cost. One of the most effective ways to reduce the cost of water-holding materials is the use of cheap fillers, which can also significantly modify the consumer properties of the copolymers and to be more the positive power supply of the plants.

Known crosslinked acrylic copolymers to increase water retention and structuring soil in gardening and agriculture.with. 1481326, the patents of the Russian Federation 2015141, 2074200, 2089561) based on acrylic acid, its salts and acrylamide. As cross-linking agents are allyl derivatives of cellulose, N,N'-methylene-bis-acrylamide, derivatives of diacrylates, cobalt salts. Polymeric materials obtained by the methods of these patents provide a high level of water absorption of up to several hundred grams of water per 1 g of dry polymer. However, achieved a high degree of water absorption lead to lower physical-mechanical characteristics of the swollen water-absorbing material, which significantly reduces its effectiveness in its use in soil with increasing depth of backfill materials is sharply reduced their degree of water absorption is more rapid destruction of the material, there is a need of additional contribution.

A method of obtaining filled acrylic copolymer based on acrylic acid (AA), ammonium acrylate (AKAM), styrene (St) and aluminasilica silicate as superabsorbent for combined and structuring of soils in agriculture (patent RU 2128191 C1, CL C08F 220/06, 1990). This copolymer contains filler aluminasilica silicate in the amount of 0.13 and 10.3 wt.% from the suits. Getting filled material is carried out by copolymerization of acrylic copolymers and Art in the presence of 20% aqueous ammonia solution, potassium persulfate and aluminasilica silicate at a temperature of 100-120°C. the Disadvantage of this method is the low degree of filling, declared the operation of washing the obtained ternary copolymer. The disadvantages also include the need for disposal of wash water containing a mixture of toxic residual monomers, and disposal of toxic fumes of nitrogen compounds using aqueous solutions of ammonia during copolymerization at higher temperatures.

The closest to the technical nature of the claimed invention is a method of obtaining full leganabatho soil conditioner (patent RU 2189382 C2, CL C09K 17/40, 2002), based on the technology of simultaneous mixing of acrylic monomers with a filler, a crosslinking agent, the components of the initiating system and further polymerization of the mixture.

Polymer-based prototype is an acrylic copolymer obtained by radical copolymerization of acrylamide, acrylic acid and of ammonium acrylate. As the filler used bentonite or palygorskite clay in the form of a fine powder in a mass ratio of monomer : clay filler is from 1:0.25 to 1:1,. Way to obtain is the mixture of monomers and fillers until a homogeneous, aggregately stable dispersion system, then enter the initiators of polymerization (potassium persulfate and sodium metabisulfite). The induction period before polymerization from 5 minutes to 1 hour. The duration of polymerization from 1 to 4 hours at a temperature of from 35 to 90°C. Then the obtained gel is crushed into small pieces, subjected to processing with an aqueous solution of potassium hydroxide at a temperature of 80÷90°C for 30 min, dried in a belt dryer and milled.

The disadvantage of this method is the use of a filler capable of swelling in an aqueous environment, resulting in greatly increasing the viscosity of the composition. The high viscosity of the composition is in the implementation process in the reactor, a large amount does not guarantee uniform distribution of components and, accordingly, voproizvodit the proposed method of obtaining the composition and characteristics of the end product or results in a significant increase mixing time to obtain a homogeneous composition.

Object of the invention is the creation of a composite water-retaining material with low cost, availability of additional sources of plant nutrition, simplification of manufacturing technology filled gel when SOH is Anenii odosobnionych properties on the level of filled and unfilled counterparts.

The problem is solved due to the fact that in the proposed method, a filler, a mixture of solid waste biocatalytic production of acrylic monomers (acrylamide and of ammonium acrylate and salts of humic acids in the form of an aqueous paste in the ratio 99/70÷1/30 wt.% on the dry substance, in an amount up to 60 wt.% from the amounts of monomers in terms of dry weight, is mixed with aqueous solutions of acrylamide and salts of acrylic acid (ammonium or potassium) in a ratio of 20/80 to 80/20 (mole percent), cross-linking agent in the amount of 0.10÷1.00 mole.% from the amounts of monomers and polymerization initiators (ammonium persulfate (potassium and sodium sulfite) in the amount of 0.10÷2.00 mole.% each of the sum of the monomers and then polymerized for 20÷60 minutes. The filler can be used in the form of an aqueous paste or dry powder form.

The invention consists in the following. In a cylindrical reactor with jacket water circulation on the side surface, equipped with a mixing device, loaded aqueous solution of acrylamide (AA) and a crosslinking agent N,N'-methylen-bis-acrylamide (MBAA) in the amount of 0.10÷1.00 mole.% from the amounts of monomers, which are shuffled within 5÷30 minutes until complete dissolution of the cross-linking agent. Further, when mixing the injected aqueous solutions of salts of acrylic acid (AA): ammonium acrylate (AKAM) or acrylic is potassium (ACC). The ratio of acrylamide and salts of acrylic acid 20/80 to 80/20 (the mole.%). Then added filler, a mixture of solid waste biocatalytic production of acrylic monomers (acrylamide and of ammonium acrylate and salts of humic acids in the form of an aqueous paste in the ratio 99/70÷1/30 wt.% on the dry substance, in an amount up to 60 wt.% from the amounts of monomers in terms of dry weight. Is mixing the components until a homogeneous dispersion system (temperature 10÷25°C, mixing time 3÷30 min). After entering the initiator ammonium persulfate (PSA) and sodium sulfite (SN) in an amount of 0.10÷2.00 mole.% each of the amount of monomers and stirring for 3÷15 minutes, the stirrer is switched off. The duration of polymerization of 20÷60 minutes, and thereafter discharging the obtained gel-like composite material, its crushing, drying, crushing and sieving known methods.

The main filler are solid waste biocatalytic production (TOBC) of aqueous solutions of acrylamide and of ammonium acrylate, representing gustavasson legalisierung mass, composed of individual cells, cell aggregates and auxiliary filtering mineral materials in existing industrial processes after washing of the residual monomers, for example, the disposal are stated. Advantage TALK before bentonitovykh clays is the lack of ability to swell, that is, to a sharp increase in the viscosity of the composition at the input of the filler in a solution of monomers, which reduces the time of mixing of the composition and reduce the entire production cycle of the receiving soil vlagooborote.

Additional filler is a pasty mixture of salts of humic acids (ha), which, in addition, what are structurename soil and increase crop yields, improve the stability of humified gels to biodegradation.

The filler can be used in paste form, and in a dry powder form. For that fillers pre-mixed, dried and crushed. The powdered form can reduce mixing time up to 3÷15 minutes to obtain a homogeneous composition, and the total time of receipt of filled acrylic copolymer, and increase vegasonline properties of the final product.

The resulting polymeric material filled with the solid waste production of acrylic monomers and salts of humic acids, has a network structure and can absorb 400÷750 grams of water per 1 gram of dry polymer. This allows you to use it as a water-holding material, not inferior in vegasonline its the properties of existing analogues, used in agriculture, gardening urban and industrial landscapes, as well as to strengthen the soil.

This invention is represented by the following examples.

Example No. 1.

In a glass reactor of 1 liter of mixed 149,1 g of aqueous 30% solution of acrylamide and 0.2 g MBAA is stirring for 15 minutes until complete dissolution of the powder. Enter 260,3 g of a 21% aqueous solution of ammonium acrylate and with constant stirring entered 29,2 g TALK and 12.5 g of GC on the dry substance in paste form. After 30 min stirring (after a homogeneous suspension control visual) is the input of aqueous solutions of initiators (0,57 g of ammonium persulfate and 0.31 g of sodium sulfite in aqueous solutions). After stirring for 3 minutes, the stirrer is switched off. Curing time 20 minutes. Then be cutting the obtained gel, followed by drying with hot air to solid state and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 2.

Obtaining a composite material is carried out analogously to example No. 1. It is mixed in a cylindrical metal reactor 892,8 g of 30% solution of acrylamide and 2.3 g MBAA for 5 minutes, added 1558,8 g of a 21% solution of the acrylate is ammonium. Then we introduce the fillers in the amount of 265,1 g TALK and 2.7 g / CC of dry matter in the dry powder form, mixing of the composition is carried out for 3 minutes. Then entered the initiators of the DOG and SN in the amount of 3.4 g and 1.9 g respectively in the form of aqueous solutions. Mixing time is 15 minutes. At the end of polymerization (40 minutes) cutting gel product, drying, grinding and sieving.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 3.

Obtaining a composite material is carried out analogously to example No. 1, except for using potassium acrylate instead of ammonium acrylate. Hitch humidity 131.6 g of 30% aqueous solution of acrylamide is mixed with 0.34 g of a crosslinking agent MBAA under stirring for 30 minutes to obtain a clear mixture. After entering 284,7 g of a 21% solution of potassium acrylate and fillers in the amount of 31.3 g TALK and 13.4 g of GC on the dry substance in paste form is stirring this mixture for 30 minutes, injected 2.5 g DOG and 1.4 g of SN in the form of aqueous solutions. Mixing time is 15 minutes, polymerization is 60 minutes, followed by cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1

Example No. 4.

Obtaining a composite material is carried out analogously to example 1 by mixing of 55.5 g of 30% aqueous solution of acrylamide and 0.5 g of MBAA. After 30 minutes of mixing is introduced 387,8 g of a 21% aqueous solution of ammonium acrylate, and then 50.0 g TALK and 8.8 g of ha in the dry powder. Further stirring for 15 minutes, entered 1.3 g DOG and 0.7 g of SN in the form of aqueous solutions. Mixing time is 5 minutes, polymerization is 60 minutes, followed by cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 5.

Obtaining a composite material is carried out analogously to example No. 1. 110,8 g of 30% aqueous solution of acrylamide is mixed with 1.8 g of a crosslinking agent MBA with stirring for 25 minutes to obtain a clear mixture. After entering 290,1 g 21% solution of ammonium acrylate, fillers are injected in amounts to 39.6 g TALK and 17.0 g of GC on the dry substance in paste form. Further stirring for 3 minutes, entered 5,2 g DOG and 2.9 g of SN in the form of aqueous solutions. Mixing time is 5 minutes, polymerization is 20 minutes, followed by cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are given in tables is 1.

Example No. 6.

Obtaining a composite material is carried out analogously to example No. 1, except for using potassium acrylate instead of ammonium acrylate. 252,5 g of 30% aqueous solution of acrylamide is mixed with 2.9 g of a crosslinking agent MBAA under stirring for 30 minutes to obtain a clear mixture. After entering 99,5 21% solution of potassium acrylate and fillers in the amount of 41.7 g TALK and 22.4 g of GC on the dry substance in paste form is stirring for 30 minutes, entered 5.7 g of PSA and 3.2 g of SN in the form of aqueous solutions. Mixing time is 15 minutes, polymerization is 20 minutes, followed by cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 7.

Obtaining a composite material is carried out analogously to example No. 1 in a glass reactor with a volume of 5 l 704,8 g of 30% aqueous solution of acrylamide is mixed with 7.6 g of a crosslinking agent MBAA under stirring for 30 minutes to obtain a clear mixture. After entering 820,6 g of a 21% solution of potassium acrylate fillers are injected in the number of 54.1 g TALK and 23.2 g of GC in pasty form. Further stirring for 30 minutes, enter 11.2 g of PSA and 6.2 g of SN in the form of aqueous solutions. Mixing time is 15 minutes, polymerization is 60 minutes, after which production is out cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 8.

Obtaining a composite material is carried out analogously to example No. 1, except for using potassium acrylate instead of ammonium acrylate. of 46.7 g of 30% aqueous solution of acrylamide is mixed with 0.3 g of a crosslinking agent MBAA under stirring for 20 minutes to obtain a clear mixture. After entering 404,0 g 21% solution of potassium acrylate are introduced fillers in the amount of 44.5 g TALK and 14.8 g of GC on the dry substance in powdered form. Then stirring for 25 minutes, introduces 1.1 g DOG and 0.6 g of SN in the form of aqueous solutions. Mixing time is 15 minutes, polymerization is 60 minutes, followed by cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 9. Obtaining a composite material is carried out analogously to example No. 8, except for the use of fillers in a pasty form.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Example No. 10.

Obtaining acrylic composite material is carried out in a reactor made of stainless steel with the planet is Noah mixer with a volume of 5 L. It is mixed 2449,8 g of 30% aqueous solution of acrylamide and 9.9 g MBA after stirring until complete dissolution within 30 minutes cross-linking agent is download 1098,1 g of a 21% aqueous solution of ammonium acrylate, fillers in the amount of 521,4 g TALK and 57.9 g of GC on the dry substance in paste form. After 30 minutes stirring load of 29.5 g of a DOG, and 16.3 g of SN in the form of aqueous solutions. Then the stirring 15 minutes, and polymerization for 60 minutes, followed by cutting, drying and grinding.

Characteristics of the obtained powdery composite water-retaining material are shown in table 1.

Table 1
The claimed featuresExample No. 1Example # 2Example # 3Example No. 4Example No. 5Example No. 6Example No. 7Example No. 8Example No. 9Example No. 10Example prototype
The ratio of AA/ salt AK50/50 AA/AKAM50/0 AA/AKAM 50/50 AA/ACC20/80 AA/AKAM40/60 AA/AKAM75/25 AA/ACC60/40 AA/AKAM20/80 AA/ACC20/80 AA/ACC80/20 AA/AKAM100/0
MBA, mole.% from ΣM0,10,20,20,31,01,51,00,20,20,5of 0.025-0.15
Filler: the weight.% from ΣM4245456060652060606060
The ratio of the proposed fillers TALK : GK (wt.%)70/3099/170/3085/1570/30 65/3570/3075/2575/2590/10Bentonite clay
Initiator: the mole.% from ΣM0,20,21,00,52,02,01,00,50,51,01,5
Water absorption, g/g455590620710400250460750680400300-640

1. Composite water-retaining material, based on acrylic copolymer and a filler, wherein the acrylic copolymer is made on the basis of acrylamide and salts of acrylic acid with a ratio of 20/80-80/20 mol.% in the presence of a crosslinking agent N, N'-methylene-bis-acrylamide in the amount of 0.10 to 1.00 mol.% from the amounts of monomers and polymerization initiator selected from the persulfate is potassium or ammonium and sodium sulfite in an amount of 0.10 to 2.0 mol.% each of the sum of the monomers, where the filler is used the mixture of waste biocatalytic production of acrylic monomers and salts of humic acids at a ratio 99/70-1/30 wt.% on the dry substance in the form of an aqueous paste or dry powder form, the total filler content of up to 60 wt.%.

2. A method of obtaining a composite water-retaining material comprising mixing an aqueous solution of acrylamide and a cross-linking agent N,N'-methylene-bis-acrylamide in the amount of 0.10 to 1.00 mol.% from the amounts of monomers, stirring until the complete dissolution of cross-linking agent, followed by administration of an aqueous solution of salts of acrylic acid, where the ratio of acrylamide and salts of acrylic acid is 20/80-80/20 mol.%, and filler in a dry powder form or in the form of aqueous paste, which is used as the mixture of waste biocatalytic production of acrylic monomers and salts of humic acids in the ratio 99/70-1/30 wt.% on the dry substance, in an amount up to 60 wt.% from the amounts of monomers in terms of dry weight, mixing with the subsequent introduction of the initiators of polymerization of potassium persulfate or ammonium and sodium sulfite in an aqueous solution in an amount of 0,10-2,00 mol.% each of the amount of monomers to obtain a gel and subsequent drying and grinding.



 

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3 cl, 1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: polyacryleamides are obtained by heterophase copolymerisation of vinyl monomers. First, n-dodecyclacrylamide is added to water solution of sodium dodecylsulfate, applied as stabiliser, with mixing. Then, water solution of acryleamide and acrylic acid is added to obtained dispersion. Reaction is carried out in alkaline medium at pH 9.5 with general concentration of copolymers from 3.0 to 3.8 mol/l. After that, particles of magnetic filler are added to obtained mixture with mixing in atmosphere of inert gas with gradual increase of reaction mass temperature from 20 to 55°C. Water solution of initiator, such as potassium persulphate or ammonium persulphate is added to obtained water dispersion to concentration 3.5-4.2 mmol/l. After that, obtained product is separated by known methods. As magnetic filler, applied is magnetite with particle size from 50 to 1000 nm or acicular particles of magnemite from 200 to 800 nm long with diameter from 20 to 50 nm. Magnetic liquid includes liquid phase - water or its mixture with organic solvents, such as ethanol methanol, and magnetic solid phase - upper said polyacryleamide.

EFFECT: invention makes it possible to obtain polyacryleamide by more technological economic method in absence of highly-toxic solvents and obtain magnetic liquid, which preserves sedimentation stability in magnetic field.

4 cl, 1 dwg, 1 tbl, 7 ex

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