SU1509364A1 - Method of producing water-repelling agent - Google Patents

Abstract

The invention relates to methods for the preparation of water repellents and can be used in various sectors of the national economy for treating materials in order to impart hydrophobic properties to them, in particular in construction equipment. The invention allows to simplify the process and reduce the cost of the target product. The method consists in the fact that the waste production of silicone rubber, the solubility of which in toluene is 10 - 95% (SKT, SKTVV), or waste production of rubber compounds having a plasticity of 0.1-0.7 (waste mixtures K-69, K-1520 , IRP-1400, IRP-1401, IRP-1338 and IR-21), are treated with an aqueous-alcoholic solution of alkali at 70 - 90 ° C. The weight ratio of waste: water: alkali: alcohol is 1: (1.07-1.4) :( 0.36-0.85) :( 0.53-1.0). Ethyl, propyl and isopropyl alcohols are used as alcohol. 1 tab.

Description

The invention relates to methods for the preparation of water repellents and can be used in various areas of the earth's economy for treating materials in order to impart hydrophobic properties to them, in particular in construction equipment.

The aim of the invention is to simplify the process and reduce the cost of the target product.

As waste production of silicone rubbers use waste rubber SKT, SKTV. As waste production of rubber mixtures - waste mixtures K-69, K-1520, IRP-1400, IRP-1401, IRP-1338 and IR-21. Ethyl, propyl and isopropyl alcohols are used as alcohol.

Reducing the process temperature below 70 ° C is impractical because it leads to an increase in the splitting time of the original waste, the upper temperature limit of the process is due to the boiling point of the alcohols used.

Example 1. In a flask equipped with a stirrer, a thermometer and a reflux condenser, 54 g of a 31.5% aqueous solution of KOH (where 37 g, KOH 17 g), 16 g of ethanol and 30 g of finely chopped rubber IWP waste are loaded. -1400 with ductility of 0.3. Cleavage is carried out at.

SL

About CD SO O

70 ° C for 12 hours, i.e. to complete

ten

15

degradation of the rubber compound. The mass ratio of the waste silicone rubber mixture: H20: KOH: C H OH 1: 1.23: 0.5650.53. In the resulting water-alcohol solution, the content of KOH,%: found to 16.9; calculated 17.0, the density of 1,1009 g / cm, the silicon content of 11.86 wt.%.

Example 2 Analogously to Example 1, at 70 ° C, splitting 90 g of K-69 rubber waste with a plasticity of 0.25 162 g of a 31.5% aqueous solution of NaOH (where 111 g, NaOH 51 g) and 48 g ethyl alcohol. The mass ratio of waste rubber mixture: H20: NaOHsC H OH 1: 1.23: 0.56: 0.53. In the resulting water-alcohol solution, the NaOH content,%: I7.0j was found, 17.0 was calculated, the density was 1.1100 g / cm%, the silicon content was 12.56 wt%;

Example 3. Analogously to Example 1, at 90 C, 30 g of K-69 rubber compound wastes were split with a plasticity of 0.6 to 62.5 g of a 40.8% aqueous NaOH solution (where U, 0 37 g, NaOH 25 , 5) and 16 g of propyl alcohol. The mass ratio of waste rubber compound: H2 0: KaON: C5NuOH - - 1: 1.23: 0.85: 0.53. In the resulting aqueous-alcoholic solution, the content of NaOH,%: found 22.9; calculated

 In the resulting water-alcohol solution, the NaOH content,%: found, 11, .8, was calculated 12.0, the density of 1, 0011 g / s, the silicon content was 14.85 wt.%. Example of a similar procedure to example 1, at 90 ° C 90 g of K-I520 rubber compound waste with 0.4 plasticity split 144 22.9% aqueous solution of NaOH (where 111 g, NaOH 33 g) and. g of propyl alcohol O Mass ratio waste re-mixture: NaOH: propyl alcohol 1: 1.23: 0.36: 0.73. In the resulting water-alcohol solution, the content of NaOH,%: found 10.8; calculated 11.0, density 1.0233 g / cm, silicon content 12.38 mas%

Example 7. Analogously to Example 1, at 75 ° C, splitting is carried out. 27 g of waste rubber IP-21 vulcanizates with a plasticity of 0.1 59.4 g of 36.4% aqueous solution of NaOH (where 37.8 g of NaOH is 21.6 g and 27 g of isopropyl alcohol is vulcanizates:: isopropyl alcohol 1.0:: 1.4: 0.8: 1.0. In the resulting water-alcohol solution, the content of NaOH,%: found 18.0; calculated 19.06, density 1.0254 g / cm, the silicon content of 10.78 wt.%.

Example 8. Similar to when 20

thirty

23.5, the density of 1.1410 g / cm, containing 35 1 at 90 ° C, silicon is split by 11.12% by weight of 140 g of vulcanizate wastes reexample 4oP according to the procedure similar to example 1, at 75 ° С splitting 90 g of waste rubber compound IRP-1401 with plasticity of 0.5– 165 g of 40% aqueous KOH solution (where 99 g, KOH 66 g) and 75 g of isopropyl alcohol are carried out. The mass ratio of waste-rubber mixture:: KOH: isopropyl alcohol 1: 1.1: 0.73: 0.83. In the resulting water-alcohol solution content. KOH,%: found 19.5; calculated 20, the density of 1.0357 g / cm, the silicon content of 11.14 wt.%.

Example 5o In accordance with the above procedure, at 75 C, 90 g of rubber waste RPI-1338 with a plate-size of 0.7 split 135 g of a 26.7% aqueous solution of NaOH (where 99 g, NaOH 36 g) and 75 g of isopropyl alcohol. The mass ratio of rubber waste: HjO: isopropyl alcohol - I: 1.1: 0.4: 0.83

 :

 In the resulting water-alcohol solution, the content of NaOH,%: found, 11, .81, was calculated 12.0, the density was 1, 0011 g / s, the silicon content was 14.85 wt.%. An example of a similar procedure to example 1, at 90 ° C. 90 g of K-I520 rubber compound waste with 0.4 plasticity split 144 g of a 22.9% aqueous solution of NaOH (where 111 g, NaOH 33 g) and. g of propyl alcohol about Mass respectively. wearing a waste mixture: NaOH: propyl alcohol 1: 1.23: 0.36: 0.73. In the resulting water-alcohol solution, the content of NaOH,%: found 10.8; calculated 11.0, density 1.0233 g / cm, silicon content 12.38 wt%

Example 7. Analogously to Example 1, at 75 ° C, splitting is carried out. 27 g of waste rubber vulcanizates IP-21 with a plasticity of 0.1 59.4 g of 36.4% aqueous solution of NaOH (where 37.8 g of NaOH is 21.6 g) and 27 g of isopropyl alcohol. Mass ratio of waste vulcanizates :::: isopropyl alcohol 1.0:: 1.4: 0.8: 1.0. In the resulting water-alcohol solution, the content of NaOH,%: found 18,0; calculated 19.06, density 1.0254 g / cm, silicon content 10.78 wt%.

Example 8. Similarly to

0

K-69 zine mixture 235 g of 36.1% aqueous solution of NaOH (where H, 0 150 g, NaOH 85 g) and 125 g of propyl alcohol. The mass ratio of waste vulcanizates: HgO: NaOH: propyl alcohol 1.0: 1.07: 0.6: 0.9. In the resulting water-alcohol solution. NaOH content,%: found 16.5:.

 calculated 17.0, density 1.0613 g / cm silicon content of 11.69 wt.%.

Example 9 (comparative). Analogously to example 1 with wire. d t the splitting of 30 g of rubber waste K-69 with a plasticity of 0.6 to 80 g of 40.8% aqueous solution of NaOH (where 47.4 g; NaOH 32.6 g). The mass ratio of waste rubber compound:: NaOH 1: 1.58: 1.08.

5 Splitting does not go,

 Example 10 (comparative). According to the procedure similar to Example 1, 30 g of K-69 rubber compound with plastic was disintegrated.

five .

the amount of 0.6 98 g of 32.6% alcoholic solution of NaOH. The mass ratio of waste rubber mixture: an alcoholic solution of NaOH 1: 3.06. Cleavage is not about

Example P. In the same way as in Example 1, at 70 ° С, splitting of 20 g of silicone rubber waste SKT (solubility in toluene 30%), 36.6 g of a 39.9% aqueous solution of NaOH (where H, |, 0 22 g , NaOH 14.6 g) and 16.7 g of ethyl alcohol. Mass ratio of silicone rubber waste: 41/0: NaOH: ethyl alcohol 1: 1.1: 0.73: 0.83. In the resulting water-alcohol solution, the content of NaOH,%: found, 19,8; calculated 19.9, density 1.0572 g / cm, silicon content 10.99 wt.%.

Example 12 Analogously to Example 1, at 80 ° C, the splitting of 30 g of silicone rubber SCTV waste (solubility in toluene 10%) of 53.3 g of 24.9% aqueous NaOH solution (where 40 g, NaOH 13.3 g) is carried out and 27.7 g of propyl alcohol. Mass ratio. waste silicone rubber: NaOH: propyl alcohol 1:: 1.3: 0.44: 0.92. In the resulting water-alcohol solution, the content of NaOH,%: found 12.0; calculated 12.0, density 1.0018 g / cm, silicon content 10.86 wt.%.

Example 13. According to the method, / analogous to example 1, at 75 ° C, 25 g of silicone rubber waste SCTV (solubility in 95% toluene) is decomposed with 43.5 g of a 29.9% aqueous solution of NaOH (where 30.5 g , NaOH 13.0 g) and 22.15 g of isopropyl alcohol “Mass ratio of silicone rubber waste:: NaOH:: isopropyl alcohol 1: 1.22:: 0.52: 0.9 ° In the resulting water-alcohol solution, the content of NaOH, % i found 15.0; calculated 15.6, density 1,0091 g / cm, silicon content 11.45 masdoo

The table shows the comparative data on the water-repellent ability of water repellents; clay bricks are subjected to hydrophobization.

09364

For this, 3-5% solutions are prepared. hydrophobic liquid in water ". The hydrophobic solution was uniformly applied with a brush to the surface of the brick, after which the sample was held in air for 1.5-2 hours, and then the water absorption was determined. The water absorption of Q Q bricks is determined according to GOST. For this purpose, five samples of bricks are dried at 100-110 ° C to a constant weight and weighed after cooling with an accuracy of 1 g. Samples are placed

J5 in a jar of water in one row on the lining so that the water level above the brick should be at least two centimeters and no more than ten centimeters. The samples are kept in water for 48 hours at

20 .201: After that, the samples are removed from the vessel, wiped with a damp cloth and each sample is weighed. The mass of water flowing out of the brick in the process of weighing includes

25 per mass of water-absorbed sample. The weighing time is no more than 5 minutes after the sample is removed from the water. Mass absorption is calculated by the formula

° W .100%,

t,

where t is the mass of the sample, saturated

water, g; 35 weight of dry sample,

Water absorption is defined as the average of 5 results. Formula inventions

40 A method of producing a water repellent by treating organosilicon compounds with an aqueous-alcoholic solution of alkali when heated, characterized in that, in order to streamline the process and reduce the cost of the target product, organosilicon rubbers are used as organosilicon compounds

50 with a solubility in toluene of 10-95% or waste from the production of rubber compounds with plasticity of O, 1-0.7, while the mass ratio of waste:: water: alkali: alcohol is 1:

55: (1.07-1.4) :( O, 36-0.85) :( O, 53-1.0),, and the process temperature is. 70-90 ° C

Claims (1)

Claim . ί 40 A method of producing a water-repellent agent by treating organosilicon compounds with an aqueous-alcoholic alkali solution by heating, characterized in that, in order to simplify the process and reduce the cost of the target product _? as organosilicon compounds use wastes from the production of organosilicon rubbers 50 with a solubility in toluene of 10-95% or wastes from the production of rubber compounds with plasticity of 0.1-0.7, while the mass ratio of wastes:: water: alkali: alcohol is 1: 55: (1.07-1.4) :( 0.36-0.85) :( 0.53-1.0), and the process temperature is ·. 70-90 ° C. ^- 1509364 ' Example The concentration of the solution, 7 " Water absorption per 48 h,% 1 5 2,8 2 3 5,6 3 5 4.3 4 3 . 2.7 5 3 3.0 6 5 8.2 7 5 4.6 8 5 4.0 AND 3 3.4 12 5 7.6 thirteen 5 4.6 The control- ny .3 6.7 GKZH-10 (by [2]) 5 2.9 The control- without processing - 22.3 The control- 1 ny (by W) 3 7.4