PL228523B1 - Method for producing paraffin emulsion - Google Patents

Description

REPUBLIC

POLAND

Patent Office of the Republic of Poland (12) PATENT DESCRIPTION ₍ i ₉₎ PL ₍ n) 228523 (13) B1 (21) Application number: 414098 ( ⁵¹ ) ^{lnt CL}

C10G 73/40 (2006.01) B01F 3/08 (2006.01) C08L 91/08 (2006.01) (22) Date of notification: 22/09/2015 (54)

Method for producing a paraffinic emulsion (73) The holder of the patent:

INSTITUTE OF HEAVY ORGANIC SYNTHESIS BLACHOWNIA, Kędzierzyn-Koźle, PL POLWAX SPÓŁKA AKCYJNA, Jasło, PL (72) Inventor (s):

(43) Application was announced:

27.03.2017 BUP 07/17 (45) The following was announced about the grant of the patent:

30/04/2018 WUP 04/18

JAN GNIADY, Kędzierzyn-Koźle, PL JOLANTA IŁOWSKA, Kędzierzyn-Koźle, PL BARTŁOMIEJ BERESKA, Gliwice, PL MICHAŁ SZMATOŁA, Katowice, PL RAFAŁ GRABOWSKI, Siemianowice Śląskie, PL BRONISŁAW DEJNEGA, PL Kędzierzyn-Koźle, PL Kędzierzyn-Koźle, PL

JOLANTA BUBICZ, Kędzierzyn-Koźle, PL WITOLD HAAS, Kędzierzyn-Koźle, PL RENATA KUBICA, Bierawa, PL RENATA FISZER, Kędzierzyn-Koźle, PL IZABELA ROBAK, Chorzów, PL GRZEGORZ KUBOSZ, Czechowice-JasłoKOW, PL IWONA, PL IWONAKOWSKA , (74) Representative:

thing, pat. Renata Fiszer co

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PL 228 523 B1

Description of the invention

The subject of the invention is a method of producing a paraffinic emulsion for impregnating paper intended primarily for contact with food.

Emulsions are used in many industries, such as cosmetics, pharmaceutical, agricultural, food, pesticides, textile, polymer, construction, paints and varnishes, paper, leather processing, mining, electroplating, protective, petrochemical and cleaning agents. Water-based wax emulsions are used in the production of cosmetics, pharmaceuticals, the food industry, the textile industry, construction, paper industry and protective agents. The packaging is a barrier between the product and external factors, the main function of which is to maintain adequate protection of the content, especially if it is a food product. In order to improve the protective properties of packaging, it is recommended to impregnate them. Impregnations should be water-resistant, easy to apply, as low as possible and, above all, safe to use. The coating agent for food cartons should provide adequate barrier properties against the penetration of undesirable substances from the packaging itself into the food. The results of many studies confirm the possibility of migration to food of potentially harmful substances from packaging, especially made of recycled cardboard (Jurek, A .; Leitner, E. Food Additives & Cantaminants: Part A, 2015, O'Connor, G .; Hudson, N .; Buckley, S. Pack. Technol. Sci. 2015, 28, 75-79 Arvanitoyannis, I .; Bosnea, L. Crit. Rev. Food Sci. 2004, 44, 63-76, Lamberti, M .; Escher , F. Food Rev. Int. 2007, 23, 407-433 As research has shown, even multilayer polyethylene-aluminum laminates of the Tetra Pak type are not completely protected against migration.

Currently, varnishes, waxes and layers of thermoplastic polymers are used as impregnations for food packaging. The high hydrophobicity of these coatings prevents effective recycling of the packages covered with them due to the difficulties in removing the impregnation. Other types of protective coatings are polymer dispersions (BASF), which have good protective properties, but their cost is too high or, in the light of the EU directive and regulation 76/893 / EEC; 89/109 / EEC and EC No. 1935/2004, are not suitable for contact with food.

Polish patent PL 196969 discloses a method of producing a hydrocarbon emulsion from slack wax and / or paraffin, characterized in that water, preferably demineralized, in the amount of 300-660 parts by weight, decahydrate borax in the amount of 0.1-20 parts by weight, diethanolamine and / or monoethanolamine and / or triethanolamine in the amount of 0.1-4 parts by weight and diesel oil and / or paraffin oil and / or vaseline oil in the amount of 0-20 parts by weight are heated at a temperature of 60-100 ° C and mixed until a homogeneous mixture is obtained then gradually introduced into the reactor, which has 700-900 parts by weight of slack wax and / or paraffin with 15-75 parts by weight of stearin at the temperature of 65-100 ° C, the whole is heated to 65-100 ° C with stirring. C until a homogeneous mixture is obtained, then an aqueous solution of ammonia in the amount of 0-10 parts by weight, based on 100% ammonia, and diesel oil and / or paraffin oil and / or vaseline oil in the amount of 0-2 0 parts by weight, the whole is stirred at a temperature of 60-100 ° C for 0.05 to 2 hours, then the obtained mixture is directed to the pump, where the mixture is forced through a homogenizing valve operating at a pressure of 2-30 MPa, then the mixture is expanded and cools.

In the Polish application P. 411776 a method of preparing a paraffin emulsion is presented, characterized in that at a temperature of 80-99 ° C 80 parts by weight of paraffin, 3-10 parts by weight of stearin and 0-15 parts by weight of glycerin monostearate are mixed until a homogeneous mixture is obtained, then a solution containing 0.1-5 parts by weight of monoethanolamine and / or diethanolamine and / or triethanolamine, 0.1-0.8 parts by weight of sodium hydroxide in 50-200 parts by weight of water is gradually dosed so that the temperature in the reactor does not drop below 85-90 ° C, the contents of the reactor are stirred at a temperature of 90-99 ° C and stirred for another 10-60 minutes, then the mixing is turned off, the whole is left for several minutes for preliminary deaeration, then subjected to two-stage homogenization, passing it through a high-pressure homogenizer at a pressure of 5-60 MPa in the first homogenization stage and a pressure of 0.1-10.0 MPa in the second homogenization stage.

The object of the invention was to provide a simple and economical method of producing a paraffinic emulsion for impregnating paper intended for contact with food.

PL 228 523 B1

It has turned out that on the basis of paraffin, stearin, glycerin monostearate and / or ethoxylated sorbitan monostearate and / or sorbitan monostearate and / or ethoxylated sorbitan monooleate and / or sorbitan monooleate, sodium hydroxide and water it is possible to develop an uncomplicated and economical process. paraffin emulsion for impregnating paper intended for contact with food.

The essence of the process according to the invention is that at a temperature of 80-99 ° C, 100 parts by weight of petroleum and / or synthetic paraffin 2-10 parts by weight of stearin and 5-15 parts by weight of glycerol monostearate and 0-5 parts by weight of ethoxylated sorbitan monostearate , 0-5 parts by weight of sorbitan monostearate, 0-5 parts by weight of ethoxylated sorbitan monooleate and 0-5 parts by weight of sorbitan monooleate are mixed until a homogeneous mixture is obtained, then a solution containing 0.2-1.0 parts by weight of sodium hydroxide is gradually dosed in 60-250 parts by weight of water so that the temperature in the reactor does not drop below 85-90 ° C, then the contents of the reactor are stirred at 90-99 ° C for another 10-60 minutes, then the stirring is turned off and the whole is left to stand. for several minutes in order to pre-deaerate, undergo at least once a two-stage homogenization, passing the reactor contents through a high-pressure homogenizer at a pressure of 5-60 MPa in the first homogenization stage and at a pressure of 0.1-10.0 MPa in the second homogenization stage.

The mixing speed is preferably 250-350 rpm.

Preferably, the paraffin used is a paraffin from the Fischer-Tropsch synthesis.

Preferably, petroleum paraffin is used as the paraffin.

The paraffin is preferably a Fischer-Tropsch paraffin and a petroleum paraffin.

Preferably, the pressure used in the second homogenization stage is several times lower than in the first homogenization stage.

Preferably ethoxylated sorbitan monostearate is used as the emulsifier.

Preferably, sorbitan monostearate is used as the emulsifier.

P r z k ł a d 1

To a glass reactor having a nominal volume of 2.5 dm ³ provided with a heating mantle, a thermocouple, reflux condenser, variable speed stirrer is charged with 50 g of paraffin LTP56 / 25 production Lotus paraffins Jasło, 50 g of paraffin synthetic Sarawax SX70, 5 g of stearin, 10 g glycerol monostearate and 2 g ethoxylated sorbitan monooleate. The mixture is heated to 95 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 45 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 120 g of distilled water is introduced into the resulting mixture. It is heated and stirred at 93-95 ° C for 21 minutes. After this time, the mixture was left for 12 minutes, after which the obtained emulsion was homogenized by passing it through the homogenizer at a rate of liters / hour, at a pressure of 16 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 52 ° C.

A homogeneous, flowable, very viscous emulsion is obtained, pH 9.4, 47% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) of 2500 mPas.

P r z k ł a d 2

50 g of LTP56 / 25 paraffin, 50 g of Sarawax SX70 paraffin, 5 g of stearin, g of glycerin monostearate and 2 g of sorbitan monooleate are introduced into the reactor. The mixture is heated to 93 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 45 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 120 g of water was introduced into the resulting mixture. It is heated and stirred at 93-94 ° C for 21 minutes. After this time, the mixture is left for 15 minutes, the resulting emulsion is homogenized by passing it through a homogenizer at a speed of 9 liters / hour, a pressure of 20 MPa for the first homogenization stage and a pressure of 3 MPa for the second homogenization stage. After homogenization is complete, the sample is cooled to 52 ° C.

A homogeneous paste with a pH of 9.5 is obtained, containing 50% dry matter.

PL 228 523 B1

P r z k ł a d 3

50 g of LTP56 / 25 paraffin made by Lotos Parafiny Jasło, 50 g of Sarawax SX70, 5 g of stearin, 10 g of glycerin monostearate and 2 g of sorbitan monostearate are introduced into the reactor. The mixture is heated to 90 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 47 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 120 g of water was introduced into the resulting mixture. It is heated and stirred at 94-96 ° C for 22 minutes. After this time, the mixture was left for 13 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour, at a pressure of 16 MPa in the first homogenization stage and a pressure of 2 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 50 ° C.

A homogeneous, flowable, very viscous emulsion is obtained, pH 9.1, 51% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) 1700 mPas.

P r z k ł a d 4

50 g of LTP56 / 25 paraffin by Lotos Parafiny Jasło, 50 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerol monostearate and 2 g of ethoxylated sorbitan monostearate are introduced into the reactor. The mixture is heated to 94 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 49 minutes). A solution at 86 ° C. containing 0.8 g of NaOH in 120 g of distilled water is introduced into the resulting mixture. It is heated and stirred at 95-97 ° C for 20 minutes. After this time, the mixture was left for 14 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour, at a pressure of 16 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 52 ° C.

A homogeneous emulsion with the consistency of a thick cream and a pH of 9.2 containing 51% dry matter is obtained.

P r z k ł a d 5

50 g of LTP56 / 25 paraffin by Lotos Parafiny Jasło, 50 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerol monostearate and 2 g of sorbitan monostearate are introduced into the reactor. The mixture is heated to 94 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 40 minutes). A solution at 86 ° C. containing 0.8 g of NaOH in 120 g of distilled water is introduced into the resulting mixture. It is heated and stirred at 93-94 ° C for 22 minutes. After this time, the mixture was left for 11 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour at a pressure of 30 MPa in the first homogenization stage and a pressure of 2 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 50 ° C.

A homogeneous emulsion with the consistency of a thick cream and a pH of 9.2 containing 51% dry matter is obtained.

P r z k ł a d 6

50 g of LTP56 / 25 paraffin by Lotos Parafiny Jasło, 50 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerol monostearate and 2 g of sorbitan monostearate are introduced into the reactor. The mixture is heated to 95 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (about 41 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 177 g of water was introduced into the resulting mixture. It is heated and stirred at 93-95 ° C for 25 minutes. After this time, the mixture was left for 11 minutes, after which the obtained emulsion was homogenized twice by passing it through the homogenizer at a speed of 9 liters / hour at a pressure of 16 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After completion of the second homogenization, the sample is cooled to 50 ° C. A homogeneous liquid emulsion is obtained, pH 9.4, 40% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) of 90 mPa · s.

P r z k ł a d 7

100 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerol monostearate and 2 g of sorbitan monostearate are introduced into the reactor. The mixture is heated to 95 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (about 41 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 177 g of water was introduced into the resulting mixture. It is heated and stirred at 93-95 ° C for 25

The time was taken for a minute. After this time, the mixture was left for 11 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour at a pressure of 13 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 50 ° C.

A homogeneous, flowable emulsion is obtained, pH = 9.5, with 41% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) of 450 mPa · s.

P r z k ł a d 8

50 g of LTP56 / 25 paraffin by Lotos Parafiny Jasło, 50 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerol monostearate, 1 g of ethoxylated sorbitan monostearate and 1 g of sorbitan monostearate are introduced into the reactor. The mixture is heated to 95 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 30 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 177 g of water was introduced into the resulting mixture. It is heated and stirred at 93-95 ° C for 25 minutes. After this time, the mixture was left for 11 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour at a pressure of 13 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 50 ° C.

A homogeneous, flowable emulsion, pH 9.5, was obtained, with 41% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) of 550 mPa · s.

P r z k ł a d 9

50 g of LTP56 / 25 paraffin by Lotos Parafiny Jasło, 50 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerol monostearate, 1 g of ethoxylated sorbitan monooleate and 1 g of sorbitan monooleate are introduced into the reactor. The mixture is heated to 95 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (about 41 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 177 g of water was introduced into the resulting mixture. It is heated and stirred at 93-95 ° C for 25 minutes. After this time, the mixture was left for 11 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour at a pressure of 13 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 50 ° C.

A homogeneous, flowable emulsion is obtained, pH = 9.5, 40% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) of 500 mPa · s.

P r z k ł a d 10

50 g of LTP56 / 25 paraffin by Lotos Parafiny Jasło, 50 g of Sarawax SX70 paraffin, 5 g of stearin, 10 g of glycerin monostearate, 0.5 g of ethoxylated sorbitan monostearate 0.5 g of sorbitan monostearate 0.5 g of ethoxylated sorbitan monooleate are introduced into the reactor and 0.5 g sorbitan monooleate.

The mixture is heated to 95 ° C while the ingredients are mixed at 300 rpm until a homogeneous mixture is obtained (approximately 20 minutes). A solution at 85 ° C. containing 0.8 g of NaOH in 177 g of water was introduced into the resulting mixture. It is heated and stirred at 93-95 ° C for 25 minutes. After this time, the mixture was left for 15 minutes, after which the obtained emulsion was homogenized by passing it through a homogenizer at a speed of 9 liters / hour at a pressure of 13 MPa in the first homogenization stage and a pressure of 4 MPa in the second homogenization stage. After homogenization is complete, the sample is cooled to 50 ° C.

A homogeneous, flowable emulsion is obtained, pH = 9.5, 40% dry weight and Brookfield viscosity (spindle # 28, 100 rpm) of 500 mPa · s.

Claims (8)

Process for the production of a paraffinic emulsion, characterized in that, at a temperature of 80-99 ° C, 100 parts by weight of petroleum and / or synthetic paraffin 2-10 parts by weight of stearin and 5-15 parts by weight of glycerol monostearate and 0-5 parts by weight of ethoxylated Sorbitan Monostearate, 0-5 parts by weight Sorbitan Monostearate, 0-5 parts The amounts by weight of ethoxylated sorbitan monooleate and 0-5 parts by weight of sorbitan monooleate are mixed until the mixture is homogeneous, then a solution containing 0.2-1.0 parts by weight of sodium hydroxide in 60-250 parts by weight of water is gradually dosed in. so that the temperature in the reactor does not drop below 85-90 ° C, then the contents of the reactor are stirred at the temperature of 90-99 ° C for another 10-60 minutes, after which the mixing is turned off, the whole is left for several minutes for initial deaeration, subjected to two-stage homogenization at least once, by passing the reactor contents through a high-pressure homogenizer at a pressure of 5-60 MPa in the first homogenization stage and at a pressure of 0.1-10.0 MPa in the second homogenization stage. 2. The method according to p. The process of claim 1, wherein the mixing speed is 250-350 rpm. 3. The method according to p. The process of claim 1, wherein the paraffin is a paraffin from the Fischer-Tropsch synthesis. 4. The method according to p. The process of claim 1, wherein the paraffin is petroleum paraffin. 5. The method according to p. The process of claim 1, wherein the paraffin is Fischer-Tropsch paraffin and petroleum paraffin. 6. The method according to p. The process of claim 1, characterized in that the pressure used in the second homogenization stage is several times lower than in the first homogenization stage. 7. The method according to p. The process of claim 1, wherein ethoxylated sorbitan monostearate is used as the emulsifier. 8. The method according to p. The process of claim 1, wherein sorbitan monostearate is used as the emulsifier.