Method of producing heat-resistant leather

FIELD: chemistry.

SUBSTANCE: method involves chrome tanning and post-tanning a semi-finished product through chrome tanning in the presence of a product of reaction of 3-aminopropyltriethoxysilane and glycidylmethacrylate in molar ratio of 1:2 and consumption of the chrome tanning agent and reaction product of 3-4% and 2-3% of the weight of the semi-finished product respectively. Neutralisation and hydrophobisation with a polymer tanning agent are then carried out for 30-40 minutes with consumption of the tanning agent equal to 8-10% of the weight of the semi-finished product. After that dyeing is carried out in the presence of a synthetic tanning agent in amount of 3-4% of the weight of the semi-finished product. Post-tanning is carried out with a plant-material tanning agent and the semi-finished product is also treated for 20-30 minutes with a product of reacting hexamethylenediamine with phosphoric acid and urea in the presence of glycerin in molar ratio of 1:3:3:0.5 respectively, in amount of 3-4% of the weight of the semi-finished product and for 20-30 minutes with organic acid in amount of 0.5-1.0% of the weight of the semi-finished product. Further, the semi-finished product undergoes greasing and re-treated for 40-50 minutes with a product of reacting hexamethylenediamine with phosphoric acid and urea in the presence of glycerin in molar ratio of 1:3:3:0.5 and consumption of 7-8% of the weight of the semi-finished product, volume ratio of 0.8-1.0 and temperature of 20-22°C. Hydrophobisation with a polymer tanning agent, dyeing in the presence of a synthetic tanning agent, post-tanning with a plant-material tanning agent, further treatment with a product of reacting hexamethylenediamine with phoshoric acid and urea in the presence of glycerin in the said molar ratio and with organic acid is carried out in one bath. Separation and drying are carried out after all operations.

EFFECT: higher water-, fungus- and heat-resistance of leather under high moisture and temperature conditions, and wide range of special types of leather.

2 cl, 3 tbl, 5 ex

 

The invention relates to methods for production of special kinds of skin and can be used in the formulation of chrome-tanned leather for Shoe uppers, operated in severe conditions of high humidity and temperature.

A known method of manufacture of heat-resistant leathers, including chrome tanning, the neutralization of the semi-finished product, dyeing, retanning vegetable tanning agent, the first stage of waterproofing polymeric tanning agent based on the polyacrylate in the amount of 2-3% by weight of cement, greasing, the second stage of waterproofing polymeric tanning agent at a flow rate of 2-3% by weight of semi-finished and further dyeing at a flow rate of the dye of 0.8-1.0% by weight of semi-finished product (EN 2194764, CL SS /1/00, SS 9/00, SS 9/04, 20.12.2002).

The closest analogue of the proposed technical solution is the way to develop heat-resistant leathers, including chrome tanning, retanning of cake mix for 1.5-2.0 h chrome tanning agent at a flow rate of 0.6-0.8%, counting on the chromium oxide, LCD 1 and a temperature of 30-35°C, neutralization, washing, dyeing, greasing and hydrophobic for 1.5-2.0 hours polymeric tanning agent based on polyacrylate in an amount of 2.5-3.0% by weight of the semifinished product in LCD 1 and the temperature of 55-60°C in the same tank, retanning vegetable tanning agent, the processing of potassium alum at the rate of 4% from the mass of the semi-finished product, distribution, and with whom the Cabinet (Reference Tanner: Technology /edited Kida. technology. Sciences Nagpalabas. - M.: Legprombytizdat, 1986. - N.218-222).

A disadvantage of the known methods are relatively low hydrophobic and planetone properties of the skin in conditions of high humidity and temperature, as well as their lack of thermal stability at high temperature effects. In addition, these methods are designed to produce only clean skin leather, with a very narrow scope.

The technical result of the invention is the expansion of the range of special types of leathers and increase their water, plesne and temperature resistance in conditions of high humidity and temperature.

This result is achieved in that in the method of manufacture of heat-resistant leathers, including chrome tanning, retanning semi-finished chrome tanning agent, neutralization, dyeing, greasing, hydrophobic polymeric tanning agent, retanning vegetable tanning agent, distributing and drying, retanning semi-finished chrome tanning agent is produced in the presence of the product of the interaction of 3-aminopropyltriethoxysilane and glycidylmethacrylate in their molar ratio 1:2 at a flow rate of chrome tanning agent and product of the interaction accordingly 3-4% 2-3% by weight of cement, hydrophobic polymeric tanning agent for 30-40 min is carried out after neutralization at a flow rate of tanning agent 8-10% by weight of the s semi-finished product, dyeing is carried out in the presence of synthetic tanning agent in the amount of 3-4% by weight of cement, the retanning of vegetable tanning agent is carried out after dyeing, after which the semifinished product is further treated for 20-30 min product of interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 in the amount of 3-4% by weight of semi-finished and within 20-30 min of organic acid in a quantity of 0.5-1.0% by weight of cement, and after fatliquoring produce re-processing within 40-50 min product of interaction of diamine with phosphoric acid and urea in the presence of glycerin in them a molar ratio of 1:3:3:0,5 at the rate of 7-8% by weight of cement, the volume ratio of 0.8-1.0 and a temperature of 20-22°C.

This hydrophobic polymer tanning agent, the dyeing in the presence of a synthetic tanning agent, retanning vegetable tanning agent, additional processing of the product of the interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 and organic acid produced in the same tank at a temperature of 40-45°C.

A distinctive feature of the proposed method is that during doubleval the I in the presence of the product of the interaction of 3-aminopropyltriethoxysilane and glycidylmethacrylate in their molar ratio 1:2 in combination with the hydrophobic polymer after neutralization tanning agent, dyeing in the presence of a synthetic tanning agent, doublepane vegetable tanning agent after dyeing, additional treatments product of interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 and organic acid in the same tank, re-processing the product of the interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 to when the claimed costs of chemical materials and process parameters occurs synergistic effect of increasing water, plesne - and heat-resistant properties of the skin in conditions of high humidity and high temperature effects.

Conducting retanning in the presence of the product of the interaction of 3-aminopropyltriethoxysilane (AGM-9) and glycidylmethacrylate (GMA) in their molar ratio 1:2, having a masking effect, allow the tanning agent fuller and deeper understanding of the structure of the dermis, firmly communicating with the functional groups of the collagen of the skin. The introduction of chrome tanning agent less than 3%, and the product of the interaction of AGM-9 GMA less than 2% does not allow quality to the retanning process, which may lead to lower temperature joining of prefabricated and water resistance of the finished leather. The introduction of them is over 4% and 3%, respectively impractical so as to further enhance the effect does not occur.

Conducting processes of waterproofing polymeric tanning agent less than 30 min at a flow rate less than 8%, the dyeing in the presence of a synthetic tanning agent is less than 3%, additional processing by the product of the interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 (further MDFMK) in an amount of less than 3% less than 20 min and the organic acid is less than 20 min in the amount of less than 0.5% at a temperature less than 40°C, and re-processing MDFMK less than 40 min at a flow rate of less than 7%, LCD less than 0.8 and a temperature of less than 20°C, will not allow to receive a heat-resistant leather with high hydrophobic and planetone properties.

Carrying out these processes at a flow rate of chemical materials and parameters stated above is impractical because of the further increase of water, plesne and temperature resistance of the skin does not occur.

As polymeric tanning agent with the waterproofing of leather used Relugan RE, Relugan RV, Relugan RF (BASF), Ecolas M (firm Boehme), YOU on THE other 2294-076-00302267-2002 and other

As a synthetic tanning agent when dyeing - Relugan D, Relugan S, Basyntan SL (BASF), Tannic HCV (firm Boehme), DFPM on THE 17-06-164-95, PCA on THE 13-7308001-389-85, and others

As vegetable tannins extracts of chestnut, Mimosa, willow, quebracho.

The product of the interaction of 3-aminopropyltriethoxysilane and glycidylmethacrylate obtained by synthesis AGM-9 (TU 6-02-724-77) and GMA (TU 6-02-1338-86) in a molar ratio of 1:2 in a continuous mode at a temperature of 105-110°C for 20-25 min in the presence of inhibitor reaction of ionol (2,6-di-tert-butyl-4-METHYLPHENOL) TU 38-101459-75 in the amount of 0.5 wt.%. Receive a product with a viscosity 92-96 MPa·s and a good solubility in water at pH 4.

The method of obtaining the product of the interaction MDFMK is as follows.

In a mixer equipped with a stirrer and an inlet for entry of reagents, put 1 mol of the diamine (TU 6-09-36-87), 3 mol of phosphoric acid (GOST 6552-80 with ISM. 1,2) and 0.5 mol of glycerol (GOST 6824-96). The resulting mixture is heated to a fluid homogeneous mass, which is added with stirring 3 mol of urea (GOST 6691-77). The mixture is then heated at a temperature of 130°C for 1.5 h until the complete cessation of gas evolution and smooth. The polymer is soluble in water, contains (IR-spectrum) urea and guanidine groups, methylene and methine fragments.

As greasing materials used ready oiling composition based on natural and synthetic fats, for example Cutipol TIS-MF (firm Boehme), Universal S, Universal, Extra, Tramal N TU 2484-052-00302267-2000, SMX-e on THE other 2484-013-222-84-995-99 and other

The method is as follows.

Semi-finished leather for Shoe upper, obtained by the standard method of production of leather, chrome tanning of different thicknesses and range for the uppers and lining from the skins to the total cattle (appr. 22.11.1983 g), after chrome tanning and planing doublenaut when LCD 1.0 to 1.5 and a temperature of 35-40°C for 60-90 min chrome tanning agent in the presence of the product of the interaction of AGM-9 and GMA in their molar ratio 1:2 at a flow rate of tanning material and product, respectively, 3-4% 2-3% by weight of the semifinished product. After washing at a temperature of 35-40°C., neutralizing the formate and sodium bicarbonate for about 50-60 min and repeated flushing at 35-40°C. to produce a water-repellency treatment for 30-40 min at the LCD of 1.0-1.2 and a temperature of 40-45°C. the polymer tanning agent at a flow rate of 8-10% by weight of the semifinished product. Then in the same tub spend dyeing for 50-60 min at a flow rate of dyes 4-5% in the presence of a synthetic tanning agent in the amount of 3-4% by weight of semi-finished and retanning within 50-60 min of vegetable tanning agent at a flow rate of 5-6% by weight of the semifinished product. Then in the same tub prefabricated further treated for 20-30 min product of interaction MDFMK in the amount of 3-4% and within 20-30 min of organic acid in a quantity of 0.5-1.0% by weight of the semifinished product. After washing at a temperature of 60-65°C, fatliquoring for 90-120 min at a flow rate of fattening materials 11-15% by weight of semi-finished and washing at a temperature of 35-40°With re-processing within 40-50 min product of interaction MDFMK in the amount of 7-8% by weight of the semifinished product, incestmom ratio of 0.8-1.0 and a temperature of 20-22°C. After distributing and drying leather trim aqueous compositions of polymers, including water dispersion of polyurethane (Patent RU 2100442, C14C 11/00, 27.12.1997).

Example 1. The semi-finished product, from raw materials rawhide average standard method, after chrome tanning and planing doublenaut for 60 min, LCD 1.5 and a temperature of 40°With a chrome tanning agent in the presence of the product of the interaction of AGM-9 and GMA in their molar ratio 1:2 at a flow rate of chrome tanning agent and product of the interaction of respectively 3% and 2% by weight of the semifinished product. After washing at 40°C, neutralization of the formate and sodium bicarbonate for 60 min and re-wash at 40°C in the same tank with LCD 1.0 and a temperature of 40°C. to produce a water-repellency treatment for 30 min polymeric tanning agent Allans M in the amount of 8%, and the dyeing in the presence of a synthetic tanning agent Tannic HCV at a flow rate of dyes 4% and tanning agent 3% by weight of the semifinished product. After 50 min in a bath impose chestnut tanning agent in the amount of 6% by weight of the semifinished product, and processing continues for 60 minutes and Then into the bowl add the product of the interaction MDFMK in the amount of 3% by weight of cement, and after 20 min - 85%solution of formic acid in the amount of 0.5% by weight of semi-finished product and processing continues for another 20 minutes After draining the bath and washing at temperatures of 60°C to produce greasing for 9 min material Cutipol TIS-MT at the rate of 11% by weight of the semifinished product. After washing at 40°To produce a second processed product of interaction MDFMK in the amount of 7% by weight of the semifinished product in LCD 0.8 and a temperature of 20°C for 40 minutes After distributing and drying leather trim aqueous compositions of polymers, including water dispersion of polyurethane.

Example 2. The semi-finished product obtained by standard methods from raw materials byczyna easy process as in example 1, but retanning chrome tanning agent in the presence of the product of the interaction of AGM-9 and GMA in their molar ratio of 1:2 produced during consumption of chrome tanning agent 3.5% and the product of the interaction of 2.5% by weight of the semifinished product. The hydrophobization 9%mi polymeric tanning agent YOU within 35 minutes, the dyeing in the presence of 3.5% synthetic tanning agent PCA, retanning, quebracho, additional processing within 25 min product of interaction MDFMK in the amount of 3.5% and processing within 25 min 50%acetic acid in the amount of 0.75% by weight of the intermediate product produced in one bath at a temperature of 43°C, and re-process the product of the interaction MDFMK in the amount of 7.5% by weight of semi-finished product is carried out at LCD 0.9 and a temperature of 21°C for 45 minutes

Example 3. The semi-finished product obtained by standard methods from raw materials byczyna heavy, treated as in example 1, but retanning chrome tanning agent in the presence of about the ukta interaction AGM-9 and GMA in their molar ratio of 1:2 produced during consumption of chrome tanning agent 4%, and the product of the interaction of 3% by weight of the semifinished product. The hydrophobization 10%polymer tanning agent Relugan'RE within 40 minutes, the dyeing in the presence of 4% synthetic tanning agent Relugan D, retanning Mimosa, additional processing within 30 min the product of the interaction MDFMK in the amount of 4% and processed within 30 min of 85%formic acid at a flow rate of 1% by weight of the intermediate product produced in one bath at a temperature of 45°C, and re-process the product of the interaction MDFMK in the amount of 8% by weight of semi-finished product is carried out at LCD 1.0 and a temperature of 22°C for 50 minutes

Example 4. The semi-finished product obtained by standard methods from raw materials rawhide easy process as in example 1, but retanning chrome tanning agent in the presence of the product of the interaction of AGM-9 and GMA in their molar ratio of 1:2 produced during consumption of chrome tanning agent is 2.5% of the product of the interaction of 1.5% by weight of the semifinished product. The hydrophobization of 7.5%polymer tanning agent YOU within 25 minutes, the dyeing in the presence of 2.5% synthetic tanning agent PCA, retanning, quebracho, additional processing within 15 min the product of the interaction MDFMK in the amount of 2.5% and processing within 15 min of 85%formic acid at a flow rate of 0.4% by weight of the intermediate product produced in one bath at a temperature of 35°C, and re-process the product of the interaction MDFMK in the amount of 6.5% by weight prefabrications with LCD 0.7 and a temperature of 18°C for 35 minutes

Example 5. The semi-finished product obtained by standard methods from raw materials byczyna heavy, treated as in example 1, but retanning chrome tanning agent in the presence of the product of the interaction of AGM-9 and GMA in their molar ratio of 1:2 produced during consumption of chrome tanning agent 4.5% and the product of the interaction of 3.5% by weight of the semifinished product. The hydrophobization of 10.5%mi polymeric tanning agent Relugan RE within 45 minutes, the dyeing in the presence of 4.5% synthetic tanning agent Relugan D, retanning Mimosa, additional processing within 35 min product of interaction MDFMK in the amount of 4.5% and processing within 35 min 50%acetic acid at a flow rate of 1.5% by weight of semi-finished product is carried out at a temperature of 50°C, and re-process the product of the interaction MDFMK in the amount of 8.5% by weight of semi-finished product is carried out at LCD 1.2 and a temperature of 25°C for 55 minutes

Indicators hydrophobic properties of the skin and skin of the prototype are presented in table 1. Tests conducted on the device HPH-2 according to GOST 938.22-71 "Skin. The method of determining vodopronitsaemosti and permeability in dynamic conditions".

Indicators of heat resistance of the obtained leather and skins for the prototype presented in table 2. Tests carried out according to GOST R 52221-2004 "non-woven Cloth. Methods for determining thermal stability and change linamarase after heat treatment".

According to GOST under heat resistance refers to the ability of a material to withstand exposure to elevated temperatures while maintaining the appearance, structure and properties.

Evaluation of thermal stability of the samples of skin were made on appearance, physical-mechanical indicators and changes in linear dimensions - shrinkage along the length (Yd) and width (YW) after heat treatment.

The resistance of samples of leather, Kτ, defined by the ratio of indicators of the breaking load before and after heat treatment according to the formula

where τ - average value of breaking load after heat treatment, H;

But the average value of breaking load before heat treatment, N.

In accordance with GOST skin is considered resistant if the value of the index of heat resistance is 90% or more.

The temperature of the welding prefabricated determined after retanning chrome tanning agent according to GOST 938.25-73 "Skin. The method of determining the temperature welding".

Pressestelle skin is determined according to GOST 9.048-85. The indices of the skin samples in the scores are: 0 - total absence of mold; 1, 2, 3, 4, 5 - the defeat of the mold surface of the sample, respectively, %: 5, 25, 50, 75 100. The test results presented in table 3.

The proposed use is th way will allow you to get water, plesne-, heat-resistant leather for the uppers, operated in severe conditions of high humidity and temperature.

Table 1
Indicators hydrophobic properties of the skin
Name of indicatorValues for the examplesThe proto-type
12345
Vodopronitsaemosti in dynamic conditions min656770606950
Permeability, g/cm2h0,30,20,20,40,2 0,5
Table 2
Indicators of heat resistance leather
Name of indicatorValues for the examplesThe placeholder
12345
Temperature welding material °C
The resistance, Kτ, % during curing for 2 min
124125126115125110
at 180°C969798939793
at 280°C959697929690
at 380°C929393909385
at 400°C899090869080
Shrinkage of the sample, the length,dwhen holding for 2 min at 380°C, %6,05,6of 5.47,05,515,5
Shrinkage of the sample width, YWwhen keeping in tip is of 2 min at 380°C, %6,56,05,87,36,020,5
The change in appearance during curing for 2 min
at 180°Cnononononono
at 280°Cnononononono
at 380°Cno nonononobloating
at 400°Cbloatingnonobloatingnoswelling and delamination

15-20°C
Table 3
Indicators of pressestelle leather
Name of indicatorValues for the examplesThe placeholder
12345
Pressestelle through 30/60 days, scores, when the holding temperature
0/00/00/00/00/00/0
20-25°C0/00/00/00/00/00/0
25-30°C0/00/00/00/00/00/0
30-35°C0/00/00/00/00/00/1
35-40°C0/00/00/00/10/01/2
40-45°C0/00/00/00/20/02/3

1. The method of manufacture of heat-resistant leathers, including chrome on the consumption, retanning of semi-finished chrome tanning agent, neutralization, dyeing, greasing, hydrophobic polymeric tanning agent, retanning vegetable tanning agent, distributing and drying, characterized in that the retanning of semi-finished chrome tanning agent is produced in the presence of the product of the interaction of 3-aminopropyltriethoxysilane and glycidylmethacrylate in their molar ratio 1:2 at a flow rate of chrome tanning agent and product of the interaction accordingly 3-4% 2-3% by weight of cement, hydrophobic polymeric tanning agent for 30-40 min is carried out after neutralization at a flow rate of tanning agent 8-10% by weight of cement, the dyeing is carried out in the presence of synthetic tanning agent in the amount of 3-4% by weight of cement, vegetable retanning the tanning agent is carried out after dyeing, after which the semifinished product is further treated for 20-30 min product of interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 in the amount of 3-4% by weight of semi-finished and within 20-30 min of organic acid in a quantity of 0.5-1.0% by weight of cement, and after fatliquoring produce re-processing within 40-50 min product of interaction of diamine with phosphoric acid and urea in the presence of glycerol when m is flax ratio of 1:3:3:0,5 at the rate of 7-8% by weight of cement, volume ratio of 0.8-1.0 and a temperature of 20-22°C.

2. The method according to claim 1, characterized in that the hydrophobic polymer tanning agent, the dyeing in the presence of a synthetic tanning agent, retanning vegetable tanning agent, additional processing of the product of the interaction of diamine with phosphoric acid and urea in the presence of glycerol when a molar ratio of 1:3:3:0.5 and organic acid produced in the same tank at a temperature of 40-45°C.



 

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