The method of obtaining the adhesion of the additive to bitumen

 

(57) Abstract:

The invention relates to the technology of building materials, for example materials used in the construction of roads (road service, road repairs). The task of the invention is to increase the efficiency of the additive for improving the adhesion properties of the additive. Additive is obtained by combining the acid component of the fatty acid or protohuman with the main component - polyethylenepolyamine at 140-180C to reach an acid number of the reaction products is not more than 25 mg KOH/g, the mixture is then cooled to 60-45C and add dibutylamino acid in an amount of 3-10 wt.%. table 1.

The technical field to which the invention relates

The invention relates to the field of technology of building materials, and more particularly to methods of producing surface-active (adhesion) of the substances used as additives to the bitumen to improve the adhesion of bitumen with mineral materials.

The level of technology

As adhesive additives to the bitumen used amidoamine, imidazoline and/or their mixtures formed during the synthesis process. Methods of obtaining adhesion additives largely defined the adhesion of bitumen and mineral materials in real conditions of use, for example, in the construction of roads.

A method of obtaining adhesion additives for bitumen multifunctional actions [1]. The method comprises combining in a reactor a mixture of polyethylenepolyamines with piperazines and a mixture of saturated and unsaturated fatty acids with long hydrocarbon radical WITH8-C26the stirring of the reaction mass with self-heating due to exothermic reaction within 2-30 minutes, the supply of inert gas (nitrogen), gradual heating of the reaction mass up to 200C for 3-4 hours, up to 240-260C for 1 h and the temperature of the reaction mass at 240-260C for 3-4 h with subsequent distillation of the excess amine at a pressure of 20-50 mm RT.article The method involves the use of a mixture of polyethylenepolyamines with piperazines of the following composition, wt.%:

Diethylenetriamine, (DETA) 25-35

Triethylenediamine (THETA) 15-25

Tetraethylenepentamine (TAP) 15-25

-Aminopiperidin (-AP) 8-12

di-Aminopiperidin (JI-AP) 5-10

The combined reaction mixtures of polyethylenepolyamines with piperazines and saturated and unsaturated fatty acids is carried out in a ratio of 1:(1,1-1,3).

As a result of implementation of the method is formed adhesion 10-20

3. AMINOETHYLPIPERAZINE 15-25, m=1, 2

4. Aminopiperidine 5-25, x=0, 1

where R is a hydrocarbon radical C15-55saturated and unsaturated fatty acids or mixtures thereof.

After the cyclocondensation reaction of the adhesion additive is characterized by an acid number 2-85 mg KOH/g and has a melting point of 45-85C.

The closest in technical essence and efficiency of adhesion is a method of obtaining a cationic adhesive additives to the bitumen, comprising combining in a reactor acidic and basic components and stirring for 1-2 hours when heated to 100-180C. as a main component according to the invention, use solutions of aminecontaining resins, and as an acid component is a mixture of synthetic fatty acid fraction WITH20and above [2]. Baseline characteristics of mixtures of synthetic fatty acids in the known method (acid number) - 70-100 mg KOH/g Mode synthesis adhesive additives in the parameters of acid number in the description of the invention is not disclosed. The stability of the adhesion additive according to the invention to a heat treatment at 160-220C.

The efficiency of known additives authorized additives in bitumen at least 1%, is sand 91-92%, with marble 92-94% (table).

The disadvantage of this method is the high consumption of additives and insufficient adhesion of bitumen to the marble and sand when used in amounts less than 1 wt.%

The invention

The task of the invention is to increase the efficiency of the additives mainly due to the increase in the adhesion of bitumen to the sand and the reduction of its consumption.

This task is solved in that the reaction of fatty acids with aminoguanidinium is carried out at a temperature of 140-180C to reach an acid number of (CZK) not more than 25 mg KOH/g (more than 85% conversion of fatty acids in amidoamine and imidazoline), then the mixture is cooled to 60-45C and add dibutylamino acid.

In the reaction at 140-180C To form predominantly a mixture amidoamine and imidazoline, which at 60-45C react with dibutylamino acid with formation of the corresponding salts. The latter provide high adhesion of bitumen with mineral materials.

As polyethylenepolyamine can be used triethylenediamine, Tetraethylenepentamine, and their mixture. As fatty acids - oleic acid, stearic acid is the possibility of carrying out the invention

Example 1. In a reactor with a stirrer and a heating load of 700 g of oleic acid with HT=196 mg KOH/g and 300 g of polyethylenepolyamine with alkalinity 149 ml of 0.1 N. Hcl and heated to 160C. In the interaction of fatty acids with polyethylenepolyamine (Pepa) ions for the formation of salts of:

RCOO-NH3[(CH2)2NH]nCH2CH2NH2,

which as a result of further transformations form amidoamine:

and imidazolin:

depth of the process on the 1st stage is characterized by an acid number (HT). HT is determined by potentiometric titration of a sample of the reaction products with a solution of caustic potash, and is expressed in mg KOH per 1 g of the product. HT characterizes the amount of unreacted fatty acid in the free state or in the form of salts with the PEP.

Under stirring for 90 min HT of the reaction mass reaches 7.5 mg KOH/g, i.e., the degree of conversion of fatty acids in amidoamine and imidazoline is 96,2%. The mass is then cooled to 45C and injected 100 g (10 wt.%) dibutylamino acid.

Receive 1060 g of the product containing predominantly (>85%) salt amidoamine and imidazoline with dibutylamino Ki

Example 2 (control)

In the conditions of example 1, the reaction mixture was heated to 100C. After 9 h HT is equal to 60 mg KOH/g Mass 3 was cooled and added 106 g dibutylamino acid. Got 1092 g of product containing about 60% salt amidoamine and imidazoline with dibutylamino acid, 20% salts of fatty acids, excessive polyethylenepolyamine free or in the form of salts - the rest

Example 3.

In a reactor with a stirrer and a heating load of 500 g floragatan HT=70 mg/g of KOH and 200 g of polyethylenepolyamine. The reaction mass is heated to 160C. After 30 min HT up to 14 mg KOH/g is Cooled the reaction mass to 60C and injected 35.5 g dibutylamino acid (5 wt.%) and receive 726 g of salt.

Example 4.

In the reactor with heating and stirring load of 500 g of fatty acids of sunflower oil with 172,5 mg KOH/g and 357 g of polyethylenepolyamine. The reaction mass is heated to 150C, after 180 min HT reaches 24,3 mg KOH/g is Cooled the reaction mass to 60C and add 82,0 g (about 10 wt.%) dibutylamino acid. Get 919 g of salt.

Example 5 (control)

In the experiment example 4 add instead dibutylamino acid 92.0 g of orthophosphoric acid. In the reaction medium is formed stekhoven Aut of 25.6 g (about 3 wt.%) dibutylamino acid. Get 852,6 g of salt.

Example 7.

In the experiment example 4 type of 16.9 grams (about 2 wt.%) dibutylamino acid. Get 843,9 g of salt.

Example 8 (control).

In the experiment example 5 type of 112.8 (12,0%) dibutylamino acid. Get 939,8 g of salt.

The test results of the adhesion properties of the additives in comparison with the prototype shown in the table.

As can be seen from the examples, the reaction takes place at temperatures below 140C leads to a significant increase in reaction time (example 2). The main product of the reaction are a salt polyethylenepolyamine and fatty acids.

In this case dibutylthiourea acid as a stronger displaces fatty acids from their salts with polyethylenepolyamine.

The resultant salt polyethylenepolyamine and dibutylamino acids are surface-active substances and will not work as an adhesive additive, and released fatty acids will be the ballast.

When the mass fraction dibutylamino acid less than 3% of the effectiveness of the additive is reduced (example 7), when the mass fraction of more than 10% is not increased (example 8).

Thus, the proposed method is avanyu with analogue.

Sources used

1. RF patent 2130954, C 08 L 95/00, publ. 1999, bull.15.

2. RF patent 2185401, CL 04 In 26/26, publ. 2002, bul.20 is a prototype.

3. RF patent 2099370, C 08 L 95/00, publ. 1997, bull.35.

The method of obtaining the adhesion of the additive to bitumen, comprising combining in a reactor acidic and basic components, the mixing by heating, characterized in that as the acid component used fatty acids or flatulate, as a main component use polyethylenepolyamine, stirring while heating is carried out at a temperature of 140-180C to reach an acid number of the reaction products is not more than 25 mg KOH/g, the mixture is then cooled to 60-45C and add dibutylamino acid in an amount of 3-10 wt.%.

 

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