The method of obtaining porous material

 

(57) Abstract:

The method of obtaining porous material includes the formation of a disperse system, the dispersed phase of which contains latex and collagen containing waste from the leather industry, subjected to titration with alkali to a pH of 10-12. According to the method, formed a disperse system is cooled to a temperature equal to 2-4°C, and then frozen at a temperature sufficient for its structure, while the saturation of the dispersed system air when the change in the average concentration of the dispersed phase in the whole volume of not more than 2%. Structured disperse system then give a defined shape and freeze it to fully cure. After thawing and drying obtain the target product of a given shape, the Method allows to obtain a material with tensile strength up to 0.25 MPa, elongation of 150%. 5 C.p. f-crystals,

The invention relates to porous polymeric materials, and more specifically to a method for producing a porous material. The invention will find application in the production of heat and sound insulation materials used in construction, machinery, footwear industry, in addition, the invention vosmoy silicone elastomer sponge with a predominantly closed-cell foam [1]. In accordance with this method, the aqueous emulsion of polyorganosiloxane (the content of which is 30-60 wt.% at pH 9-11,5 and a molecular weight of 10,000), including additional colloidal silica and the organic compound of tin, is subjected to freezing at a temperature of minus 18oC for 24 h, followed by thawing with getting wet elastic spongy material.

The formation of the spongy structure of the material is provided by the colloidal silica, which organizes the structure of the emulsion due to sorption polyorganosiloxane. It is colloidal silica and the organic compound of tin to allow drying of the obtained material to fix it a sponge-like structure. Silicone elastomeric sponge with closed pores is obtained only by drying the wet spongy material, which has a wet polymer wall then often stick together.

This method is technologically simple, its implementation is missing from toxic waste. However, it is not possible to modify the structure of the silicone sponge within wide limits depending on its application, in addition, the known method because of the influence of colloidal silica and compounds of tin drop the TEW and durability. Upon receipt of the material thickness in excess of 10-20 mm above disadvantages are amplified.

A method of obtaining a porous polymer material that obtains a polymer latex dispersion, applying the dispersion on a flexible porous fibrous substrate, the coagulation of the polymer latex by freezing and drying the obtained product [2]. Processing in a known manner is subjected to the latexes of polymers capable of coalescence at drying in the temperature range 10 - 100oC and characterized by zechusim module comprising at least 22 PA under tension by 5%. The concentration of the polymer dispersed phase in the dispersion system is 10 to 75 wt.%. Before applying the latex is infilled up to 10-40 P using casein and ammonium alginate and sodium polyacrylate. The dispersion is injected thickeners and fibrous additives. All these ingredients when applying stabiliziruyushchego factor (in this case, freezing) lead to the formation of an ordered structure in coagulation and accelerate this process, ensuring the formation of the porous polymer structure.

However, the described method does not directly regulate the porous structure and to obtain a polymeric material with a, when using a disperse system containing liquid dispersion medium capable of solidification, and a disperse phase containing synthetic latex and powdered collagen containing waste from the leather industry (100 wt.h. at 25-100 wt. o'clock, respectively), as well as vulcanizing agents [3]. According to the method specified disperse system is first frozen at (-2) - (-12)oC for 5-15 minutes until a viscous-plastic state, permitting the molding of the obtained semi-product. Semi-finished product, retaining a given shape, and then subjected to subsequent freezing is carried out at (-70 - (-8)oC for 0.5 to 6.0 hours

In the second stage freezing is complete solidification of the dispersed system and essentially completes the formation of the porous structure of the material. After the second phase of the freezing spend thawing of the material obtained and drying.

This method is technologically simple, allows to some extent to regulate the structure of the porous material and change its properties (elasticity and hardness) depending on requirements. In addition, shumaisi and other additives. However, the known method does not allow guaranteed to obtain a porous material with these characteristics. If successful, the method receiving material is not elastic, strength, residual deformation, sufficient for successful use of this material as, for example, shock absorber.

In addition, upon receipt of the material in the process of drying see significant shrinkage of the material. Acceptable physical and mechanical characteristics of only the resulting material, having a thickness of not more than 40 mm

The basis of the invention is by changing the conditions of implementation of the initial stage of freezing to develop a method of obtaining a porous material that is guaranteed to obtain the target product with a stable high physical-mechanical characteristics.

This task is solved in that in a method of producing a porous material, comprising the formation of a disperse system containing liquid dispersion medium capable of solidification, and a disperse phase comprising the latex and collagen containing waste from the leather industry, freezing educated dispiay disperse system and its freezing until complete solidification of the dispersed system, which after thawing and drying is a target product of a given shape, according to the invention, during the formation of disperse systems use named collagen containing waste, additionally previously subjected to titration with alkali to pH 10-12, while mentioned before freezing, providing structuring, the dispersed system is cooled to a temperature of 2 to 4oC, and in the process, the subsequent freezing carry out the saturation of the air dispersion system when the change in the average concentration of the dispersed phase in the whole volume of not more than 2%.

Thanks to the present method, it became possible to securely obtain a uniformly porous material of various thicknesses up to 100 mm, having a density of 1.1 g/cm3tensile strength at break of 0.25 MPa, elongation of 150%, the residual deformation of not more than 10% and a shrinkage of up to 10% (with a residual moisture content of the material constituting 10-15%). The pore size of the resulting material may be 0.1 to 2.0 mm

In accordance with the invention, it is advisable to freeze, providing structuring of a disperse system, to carry out at temperatures equal to or below -4oC, resulting in diagnosti porous material is guaranteed to desired shape appropriate, according to the invention, freezing, providing complete solidification of the dispersed system, to carry out at temperatures (-40) - (-100)oC.

To obtain material having a uniform structure and the highest values of strength, elasticity and porosity, it is expedient, according to the invention that the formed dispersion system of the dispersed phase contained 25-200 wt.h. collagen waste on 100 wt. including polymer latex.

For hardening of the structure of the material obtained by chemical means, it is expedient, according to the invention, so that in the formed dispersion system was introduced advanced vulcanizing agents in the amount of 3-10 wt.h. on 100 wt. including latex.

To create the most favorable conditions for the implementation of the freezing of a disperse system, ensuring its structuring, it is expedient, according to the invention, so that the dispersion medium additionally contained carboxymethylcellulose.

Further objectives and advantages of the invention will become apparent from the subsequent detailed description of the method of producing a porous material and concrete examples of implementation of this method.

For porous mater what food capable of crystallization, and a disperse phase comprising the latex and powdered collagen containing waste from the leather industry. Mainly the concentration of the dispersed phase is 5 to 16 wt.%. The dispersion medium is a predominantly water or aqueous solutions, including organic liquids, such as dimethylformamide. The main criterion for the choice of the dispersion medium is its ability to crystallization. Possible presence in the dispersion medium of carboxymethylcellulose, which provides regulation of the size of the ice crystals and therefore the structure of the material obtained during the initial freezing of the dispersed system.

The dispersed phase used a disperse system includes a natural or synthetic latex and collagen containing waste from the leather industry in the form of a fiber length of 0.5 to 2.0 mm. Mainly dispersed phase contains 25-200 wt.h. collagen waste on 100 wt.h. polymer latex.

When adjusting this ratio in the direction of decreasing the collagen content of the waste produced porous material can have a heterogeneous structure, which negatively affects its Phi is of the obtained porous material does not have sufficient strength.

As a source of polymer can be used polymer-containing effluents of industrial enterprises for the production and processing of latex or standard latexes, for example:

the best choice latex content of styrene units 30%,

carboxypropanoyl polibutadienovomu latex with a styrene content of links 65% and carboxyl groups 1%,

carboxypropanoyl polibutadienovomu latex content of styrene units 30% and carboxyl groups 3%,

carboxypropanoyl polybutadienes with the content of the nitrile parts of 40% and carboxyl groups 4%,

the copolymer Acrylonitrile acid with vinyl acetate,

the polyisoprene polymer natural rubber latex Qualitex.

As collagen waste the method according to the invention provides for the use of tanned and redoubling waste of skin and non-standard gelievogo raw material of the leather industry, in particular chips, obtained by equalizing the thickness of the skin, past the chrome tanning.

In accordance with the invention, collagen containing waste before using them as the basis of the dispersed phase is subjected to titration with alkali to pH 10-12, which eliminates coagulated the Tav dispersed system throughout its volume, hence, the uniform structure of the obtained material.

In addition to these substances used disperse system may contain fillers, crosslinking agents, modifiers, plasticizers and curing agents. Vulcanizing agents take as 3-10 wt.h. on 100 wt.h. polymer latex.

The use of curing agents allows chemically fix pre-formed dispersed in the polymer system structure, which will affect the strength of the resulting material.

As vulcanizing agents it is possible to use zinc oxide, sulfur, eTicket, mercaptobenzothiazole zinc, diphenylguanidine and phenyl - naphtylamine, taken in combination with each other.

Thus, to obtain a porous material in accordance with the invention, it is possible to use a disperse system of the following composition, wt%:

Collagen dispersion is 3.5

The polymer is a butadiene-styrene latex - 4,9

Zinc oxide - 0,18

Sulfur - 0,09

ETicket - 0.04

Mercaptobenzothiazole zinc - 0.04

Diphenylguanidine - 0,05

Phenyl - naphtylamine - 0.02

Water - the Rest

In accordance with the invention formed the var is the provision of a disperse system uniformly throughout its volume.

Disperse system having a temperature of 2-4oC, is subjected to freezing at a temperature sufficient for its structure, but mainly at a temperature equal to or above minus 4oC. thus, according to the invention, carried out the saturation of the air freeze dispersed system to changes in the average concentration of the dispersed phase of at most 2%. Saturation of the air is possible, for example, by bubbling through the volume of the dispersed system. The implementation of this technique facilitates the formation of the desired porous structure and its uniformity throughout the volume.

Freezing at a temperature equal to or greater than minus 4oC, is considered completed when the dispersion medium is able to maintain the vessel form, where is freezing, and at pressures up to 1 MPa does not occur of the expiration of the frozen mass of unfrozen dispersion.

The first stage of freezing is carried out in the time interval from 5 to 15 minutes of semi-product is a viscous-plastic - structured, i.e. it can take a desired shape. The first stage of freezing involves only a partial appearance of the phase contacts between the polymer particle is the same and molded with the aim of producing three-dimensional articles of predetermined shape and size. Shape with a structured intermediate quickly put then in the fridge, and implement the second stage of freezing temperatures mostly equal (-40) - (-100)oC, for 0.5 to 6.0 hours before complete solidification of the dispersed system.

After the second stage of freezing the product is subjected to thawing at room temperature. To intensify the process of removing fluid from the pore space of the material product when thawed heat. For sealing porous material defrosting can be performed at room temperature until conversion of the frozen product in a porous product, and then to subject it to pressing at a pressure of 4 to 100 MPa.

For fixing the material structure thawed product may be treated with 1% formalin solution for 1 to 8 h, after which it is washed with water at room temperature for 15-30 minutes, the resulting material may be plastifitsirovanie by immersion in 10-30% aqueous glycerin solution for 10-30 min at room temperature. In conclusion, carry out the drying of the obtained material in a heating Cabinet at a temperature of up to 40oC to remove moisture.

Received echnosti at break of 0.25 MPa; elongation at break 150%; residual deformation after repeated compression of 5%.

The study of the structure by electron microscopy showed that the resulting material has a uniform porosity, the pore size depending on the applied conditions of the method and composition of the dispersed phase may be 0.1 to 2.0 mm

These characteristics are saved in the manufacture of a porous material, having a thickness up to 100 mm

The resulting material can be successfully used as heat and sound insulation in building and industry; as a sealing or cushioning pads, parts and coatings in the manufacture of, for example, shoes.

Example 1. To obtain macroporous polymeric material using a polymer dispersion in which the polymer dispersed phase is the composition of the synthetic polymer latex in a ratio of 50 wt.h. on 100 wt. including polymer latex. Use polymer of styrene-butadiene latex with a styrene content of links 30 wt.%. The water dispersion of collagen containing material derived from waste tanned collagen chip, titrated with 0.5 M aqueous NaOH solution Is P>oC) to obtain the concentration of the polymer dispersed phase in the dispersion of 10 wt.%. The onset temperature of melting of crystals of the dispersion medium, as defined by thermogram is 0,28oC. the polymer dispersion is injected curing group: zinc oxide, sulfur, eTicket, mercaptobenzothiazole zinc, diphenylguanidine in the amount of 8.5 wt.h. on 100 wt.h. polymer latex.

8000 g of polymer dispersion at +5oC fill in the freezer, and implement the first stage of freezing at -4oC, the speed of rotation of the stirrer at 100 rpm and push the saturation of the air within 15 minutes the Process is obtaining a viscous plastic product with a concentration of dispersed phase volume 8 - 12% and containing partially crystallized dispersion medium in the form of crystalline ice, which is the germ of the future then.

The obtained semi-finished product is placed in a mold with a size of 400 x 200 x 50 and carry out the second stage of freezing and kept in a refrigerator at -40oC for 4 h (this is the complete curing of the mass with the formation of pores), and then at 10oC for 12 h

Thawing of the frozen product is carried out in the forms in to the on the porous product and drying receive the material with the following physical-mechanical properties:

The density of 1.10 g/cm3< / BR>
Tensile strength at break

Elongation of 120%

Permanent deformation - 5%

Shrinkage - 10%

Example 2. To obtain macroporous polymeric material using a polymer dispersion in which the polymer dispersion phase is the composition of the polymer natural rubber latex and collagen containing material in a ratio of 165 wt.h. on 100 wt. including polymer latex. Use natural latex Qualitex with a content of disperse phase 45 wt.%. The water dispersion of collagen containing material derived from waste Zelenih animal skins, titrated with 0.5 M aqueous NaOH solution to pH 12. Then the components of the polymer dispersion and connect with stirring, diluted with ice water to obtain a concentration of polymer of the dispersed phase in the dispersion of 5 wt. %. The onset temperature of melting of crystals dispersed environment, as defined by thermogram is -0,50oC. the Polymer dispersion contains curing group: zinc oxide, sulfur, eTicket, mercaptobenzothiazole zinc, diphenylguanidine in the amount of 8.5 wt.h. on 100 wt. including polymer latex.

8000 g of polymer dispersion at +5oC fill in the freezer and implement peruga saturated air. The final step is to obtain a viscous plastic product with a concentration of the dispersed phase in the whole volume of 3 - 7% and containing partially crystallized dispersion medium in the form of crystalline ice, which is the germ of the future then.

The obtained semi-finished product is placed in a mold with a size of 400 x 200 x 10, stand in the refrigerator at -100oC for 0.5 h (this is the complete curing of the mass with the formation of pores), and then at -20oC for 12 h

Thawing of the frozen product is carried out in the forms at room temperature until the formation of wet porous product.

After processing and drying the porous material has the following physical and mechanical characteristics:

The density is 1.2 g/cm3< / BR>
Tensile strength - 0.08 MPa

Elongation at break of 150%

The residual strain after repeated compression - 6%

Shrinkage - 15%

Example 3.

Production of porous polymeric material is carried out in conditions similar to those specified in example 1, but using a disperse system in which the polymer dispersed phase contains 200 wt.h. collagen waste on 100 wt.h. on the parts of 50%. The concentration of the polymer dispersed phase in the dispersion of 15 wt.% at pH 11. Polymer dispersion contains as a vulcanizing agent, zinc oxide in an amount of 7 wt.h. on 100 wt.h. polymer latex.

After processing and drying of porous polymeric material has the following physical and mechanical characteristics:

The density of 1.16 g/cm3< / BR>
The tensile strength

Elongation at break - 135%

The residual strain after repeated compression - 3,2%

Shrinkage - 10%

Example 4. Production of porous polymeric material is carried out in conditions similar to those specified in example 1, however, the dispersed phase further comprises a carboxymethyl cellulose in the amount of 0.5 wt.h. on 100 wt.h. polymer latex.

After processing and drying of porous polymeric material has the following physical and mechanical characteristics:

Density of 1.1 g/cm3< / BR>
Tensile strength - 0.06 MPa

The residual strain after repeated compression - 4,2%

Elongation at break - 127%

Shrinkage - 12%

1. The method of obtaining porous material, including the formation of a disperse system containing liquid h Wednesday, spavala, freezing the formed dispersion system at a temperature sufficient for its structure, followed by forming a structured disperse system and its freezing until complete solidification of the dispersed system, which after thawing and drying is a target product of a given shape, characterized in that during the formation of disperse systems use named collagen containing waste, additionally previously subjected to titration with alkali to pH 10 to 12, while mentioned before freezing, providing structuring, the dispersed system is cooled to 2 to 4oC, and in the process, the subsequent freezing carry out the saturation of the air dispersion system when the change in the average concentration of the dispersed phase in the whole volume of not more than 2%.

2. The method according to p. 1, characterized in that freezing, providing structuring of a disperse system, carried out at a temperature equal to or below minus 4oC.

3. The method according to p. 1, characterized in that freezing, providing complete solidification of the dispersed system, carried out at (-40) - (-100)oC.

4. The method according to p. 1, characterized in that obrazovan the Tex.

5. The method according to p. 1, characterized in that formed in the dispersed system to impose an additional curing agents in an amount of 3 to 10 wt.h. on 100 wt.h. polymer latex.

6. The method according to p. 1, wherein in the formed dispersion system of the dispersion medium further comprises carboxymethylcellulose.

 

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