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INVENTION
Patent of the Russian Federation RU2016016
COMPOSITION FOR ARTIFICIAL AMBER AND THE METHOD OF OBTAINING ARTIFICIAL AMBER
Applicant's name: Limited Liability Partnership "Vacancy"
The name of the inventor:
The name of the patent holder: Limited Liability Partnership "Vacancy"
Address for correspondence:
Date of commencement of the patent: 1992.05.20
Use: for the production of artificial amber, as heat-resistant coatings, composite materials, molded products. Essence: composition for artificial amber includes 100 parts by weight. A solution of polyglycol maleate terephthalate in an unsaturated monomer or oligomer; 25 to 100 parts by weight, rosin and 1 to 7 parts by weight. Succinic acid. The components of the formulation are mixed and the mixture is solidified 
- radiation at a radiation dose of 8-20 mrad and room temperature.
DESCRIPTION OF THE INVENTION
The invention relates to the production of artificial amber based on unsaturated polyester and rosin and can be used as heat-resistant coatings, composite materials, molded articles.
Natural amber is a complex mixture of organic substances, namely volatile terpenes and sesquiterpenes, soluble diterpenoids (alcohols, ethers, aldehydes, resin acids) and insoluble cross-linked polymer, which is 75-80% of the mass of amber.
For natural amber, the inconsistency of the chemical composition is characteristic. A distinctive feature of Baltic amber, succinite, and amber from other deposits is the content of significant amounts of succinic acid (3-8 wt.%).
The closest in technical essence is the composition for artificial amber, which includes a solution of polyglycolmaleinate phthalate in an unsaturated monomer or oligomer and rosin. Amber includes an initiating system - peroxide and a curing accelerator.
The method for obtaining artificial amber consists in mixing a solution of polyglycol male terminal terephthalate in an unsaturated monomer or oligomer followed by curing. The curing is carried out with an initiating system at room temperature for 90 days. A material similar in properties with natural amber is obtained (melting point, density, high gloss after polishing).
The disadvantage of the known technical solution is the duration of the curing process, the non-technological process due to the use of explosive peroxides, insufficiently high values of hardness, heat resistance, resistance to organic solvents.
The technical object of the invention is to increase the hardness, heat resistance, resistance to organic solvents, simplify the curing process.
The problem is solved by the fact that the composition for artificial amber, including a solution of polyglycol-maleate titanium phthalate in an unsaturated monomer or oligomer, and rosin, additionally contains succinic acid, with the following composition ratio, mass parts:
- A solution of polyglycol malnate-phthalate in an unsaturated monomer or oligomer 100
- Rosin 25-100
- Succinic acid 1-7
The stated task is also solved by the fact that in the process for obtaining artificial amber, consisting in mixing a solution of polyglycolmaleinate phthalate in an unsaturated monomer or oligomer and rosin, followed by curing, succinic acid is additionally used, the components of the composition are mixed and the mixture is cured -radiation at a radiation dose of 8-20 Mrad at room temperature.
According to the invention, a 40-45% solution of polypropylene glycol maleate terephthalate in styrene (resin I, grades PN-609-21), a 33-35% solution of polydiethylene glycol maleinate phthalate in styrene (resin II, grade PN-1), 45-50% (Resin III, grade PNM-2), a 42-45% solution of polyethylene glycol maleininate phthalate in triethylene glycol dimethacrylate (resin IV, grades PN-609-26), in the examples used pine rosin, can be used fir or cedar rosin.
Example 1
To 100 parts by weight Molten pine pine rosin (T razm = 68 o C, GOST 5,65-68) is added 3.6 parts by weight. Succinic acid (GOST 6341-75). The resulting homogeneous mixture is poured into a mold and irradiated with 60 Co gamma quanta to an absorbed dose of 15 Mrad (irradiation time 21 hours at a dose rate of 200 rad / s). With a yield of 98.5%, a transparent brittle material similar to rosin is obtained.
Example 2
To 100 parts by weight With molten rosin, 100 wt. H of unsaturated polyester resin PN-609-21 (TU-6-05-1306-70) - resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With a yield of 98.3%, a transparent brittle material is obtained.
Example 3
Example is similar to Example 2. As unsaturated polyester resin, PN-1 resin (MITU 6-05-1082-67) resin II is used. With a yield of 98.1%, a transparent brittle material is obtained.
Example 4
An example is similar to Example 2. As the unsaturated polyester resin, the PNM-2 resin (OST 6-05-431-78) resin III is used. With a yield of 98.0%, a transparent brittle material is obtained.
Example 5
Example is similar to Example 2. As unsaturated polyester resin, resin PN-609-26 (TU 6-05-191-92-71) resin IV is used. With a yield of 98.1%, a transparent brittle material is obtained.
Example 6
To 100 parts by weight Resin I at a temperature of 65 ° C is added with stirring 100 wt. H. Finely ground rosin to form a homogeneous mixture and 7 parts by weight. Succinic acid dissolved in 3 ml of ethyl alcohol. The resulting mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With an yield of 98.0%, an opaque solid material is obtained.
Example 7
To 100 parts by weight Molten rosin is added with stirring 7 wt. H. Succinic acid and 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With a yield of 98.4%, a clear, hard material is obtained.
Example 8
An example is similar to Example 7. Resin II is used as the resin. With a yield of 98.3%, a clear, hard material is obtained.
Example 9
An example is similar to Example 7. Resin III is used as the resin. With a yield of 98.1%, a clear, hard material is obtained.
Example 10
An example is similar to Example 7. Resin IV is used as the resin. With a yield of 98.2%, a clear, hard material is obtained.
Example 11
The example is similar to Example 7. The initial mixture is irradiated to an absorbed dose of 20 Mrad (irradiation time 28 h). With a yield of 98.7%, a clear, hard material is obtained.
Example 12
To 50 parts by weight Molten rosin is added with stirring 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 12 Mrad (irradiation time 17 h). With a yield of 98.6%, a clear, hard material is obtained which is easily processed and polished.
Example 13
To 50 parts by weight Molten rosin is added 1.5 parts by weight. Succinic acid and 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 12 Mrad. With a yield of 98.4%, a clear, hard material is obtained which is easily processed and polished.
Example 14
To 50 parts by weight Molten rosin is added with stirring 5.4 parts by weight. Succinic acid and 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 12 Mrad. With a yield of 98.4%, a clear, hard material is obtained which is easily processed and polished.
Example 15
The example is similar to Example 12. The starting mixture is irradiated to an absorbed dose of 15 Mrad. With a yield of 98.8%, a clear, hard material is obtained which is easily processed and polished.
Example 16
An example is similar to Example 15. Resin II is used as the resin. With a yield of 98.6%, a clear, hard material is obtained which is easily processed and polished.
Example 17
An example is similar to Example 15. Resin III is used as the resin. With a yield of 98.2%, a clear, hard material is obtained which is easily processed and polished.
Example 18
An example is similar to Example 15. Resin IV is used as the resin. With a yield of 98.4%, a clear, hard material is obtained which is easily processed and polished.
Example 19
To 50 parts by weight Molten rosin is added with stirring 5.4 parts by weight. Succinic acid and 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With a yield of 98.9%, a clear, hard material is obtained which is easily processed and polished.
Example 20
An example is similar to Example 19. Resin II is used as the resin. With a yield of 98.7%, a clear, hard material is obtained which is easily processed and polished.
Example 21
An example is similar to Example 19. Resin III is used as the resin. With a yield of 98.5%, a clear, hard material is obtained which is easily processed and polished.
Example 22
An example is similar to Example 19. Resin IV is used as the resin. With a yield of 98.6%, a clear, hard material is obtained which is easily processed and polished.
Example 23
To 33 parts by weight Molten rosin is added with stirring 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 8 Mrad (11 h). With a yield of 98.6%, a clear, hard material is obtained which is easily processed and polished.
Example 24
Example is similar to Example 23. The starting mixture is irradiated to an absorbed dose of 12 Mrad. With a yield of 98.7%, a clear, hard material is obtained which is easily processed and polished.
Example 25
To 33 parts by weight Molten rosin is added with stirring 1.3 parts by weight. Succinic acid and 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 12 Mrad. With a yield of 98.8%, a clear, hard material is obtained which is easily processed and polished.
Example 26
To 100 parts by weight Resin I at a temperature of 65 ° C is added, with stirring, in portions of 33 parts by weight. Finely ground rosin to form a homogeneous mixture. The mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With a yield of 98.3%, a solid opaque material is obtained which is easily processed.
Example 27
An example is similar to Example 26. Resin II is used as the resin. With a yield of 98.2%, a solid opaque material is obtained which is easily processed.
Example 28
To 33 parts by weight Molten rosin is added with stirring 100 parts by weight. Resins II. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With a yield of 98.5%, a clear, hard material is obtained which is easily processed and polished.
Example 29
An example is similar to Example 26. Resin III is used as the resin. With a yield of 98.0%, a solid opaque material is obtained which is easily processed.
Example 30
An example is similar to Example 28. Resin III is used as the resin. With a yield of 98.3%, a solid, transparent material is obtained which is easily processed and polished.
Example 31
An example is similar to Example 26. Resin IV is used as the resin. With a yield of 98.2%, a solid opaque material is obtained which is easily processed.
Example 32
An example is similar to Example 28. Resin IV is used as the resin. With a yield of 98.5%, a solid transparent material is obtained which is easily processed and polished.
Example 33
Example is similar to Example 25. The starting mixture is irradiated to an absorbed dose of 15 Mrad. With a yield of 98.9%, a clear, hard material is obtained which is easily processed and polished.
Example 34
To 33 parts by weight Molten rosin is added with stirring 1.3 parts by weight. Succinic acid and 100 parts by weight. Resins II. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 15 Mrad. With a yield of 98.6%, a solid, transparent material is obtained which is easily processed and polished.
Example 35
An example is similar to Example 34. Resin III is used as the resin. With a yield of 98.4%, a solid transparent material is obtained which is easily processed and polished.
Example 36
An example is similar to Example 34. Resin IV is used as the resin. With a yield of 98.6%, a solid, transparent material is obtained which is easily processed and polished.
Example 37
To 25 wt. H of molten rosin was added with stirring 100 parts by weight of water. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 10 Mrad (irradiation time of 14 hours). With a yield of 98.8%, a clear, hard material is obtained which is easily processed and polished.
Example 38
Example is similar to Example 37. Resin 11 is used as the resin. In a yield of 98.7%, a solid transparent material is obtained which is easily processed and polished.
Example 39
An example is similar to Example 37. Resin III is used as the resin. With a yield of 98.5%, a solid transparent material is obtained which is easily processed and polished.
Example 40
An example is similar to Example 37. As the starting resin, resin IV is used. With a yield of 98.7%, a solid transparent material is obtained which is easily processed and polished.
Example 41
To 25 parts by weight Molten rosin is added with stirring 1.0 wt. Succinic acid and 100 parts by weight. Resin I. The resulting homogeneous mixture is poured into a mold and irradiated to an absorbed dose of 10 Mrad. With a yield of 98.9%, a solid, transparent material is obtained which is easily processed and polished.
Example 42
Example is similar to Example 41. Resin II is used as the resin. In a yield of 98.7%, a solid, transparent material is obtained which is easily processed and polished.
Example 43
Example is similar to Example 41. Resin III is used as the resin. With a yield of 98.6%, a solid, transparent material is obtained which is easily processed and polished.
Example 44
Example is similar to Example 41. As the starting resin, resin IV is used. With a yield of 98.8%, a solid transparent material is obtained which is easily processed and polished.
In Table. 1 shows the elemental composition of artificial amber at different weight ratios of resin and rosin.
In the IR spectra of artificial amber (according to the invention), there are absorption bands characteristic of natural amber: 1140, 1160, 1250, 1740 cm -1 (absorption bands of stretching vibrations C = 0 and C-O-C groups of esters); 940 cm -1 (absorption band of deformation vibrations of OH carboxyl group); 1700-1710 cm -1 (vibrations C = O of the carboxyl group); 3450 cm -1 (stretching vibrations of OH carboxyl group); 885, 1410, 3090 cm -1 (the absorption bands of the valence and deformation vibrations of the C-H of the unsaturated bond of the type CR 1 R 2 = CH 2 , 995, 1420, 1660, 1800, 3090 cm -1 (absorption bands of the unsaturated bond -CH = CH 2 ), 1380, 1455, 2875, 2930 cm -1 (bands of deformation and stretching vibrations of СН in the groups СН 2 and СН 3 ).
In Table. 2 presents data on the physicochemical properties of artificial amber, depending on the conditions for its production. Radiative polymerization of pure rosin (see, example 1 of Table 2) leads to the formation of a product similar to the initial rosin for brittleness and solubility in organic solvents, but with a higher melting point. Radiative polymerization of a mixture of resin and rosin at a ratio of 1: 1 (see, example 2 of Table 2), and leads to the formation of a brittle product, but less soluble in alcohol, ether, turpentine. The introduction of succinic acid into the starting composition increases the hardness and thermal stability of the polymer product and reduces its solubility in organic solvents. According to its physico-chemical properties, this artificial amber is close to the hedanite, a variety of Baltic amber, which is more fragile (hardness 1.5-2 on the Mohs scale) and greater solubility in organic solvents compared to succinite.
As the amount of resin in the original composition increases to a resin / rosin ratio of 2: 1 (see Examples 12-22 of Table 2), a solid, transparent polymeric material is formed. The use of succinic acid as a component of the original composition increases the hardness, thermal stability, and decreases the solubility in organic solvents of the resulting polymeric material (see Examples 13, 14, 19-22 of Table 2). According to its physicochemical properties, this artificial amber is close to succinite. It is easily processed and polished.
The introduction of succinic acid into the starting composition at a resin: rosin ratio of 3: 1 and 4: 1 (see Examples 25, 33-36, 41-44) increases the thermal stability, hardness of artificial amber, and reduces its solubility in organic solvents. This composition of the mixture makes it possible to obtain artificial amber, which is close to or identical with succinite in its physico-chemical properties, and in terms of thermostability, hardness and resistance to organic solvents superior to natural amber (see Examples 33, 41).
Thus, the composition for artificial amber according to the invention and the method for its preparation allows to obtain transparent artificial amber with increased hardness, heat resistance, resistance to organic solvents, application of the radiation curing method, simplifies the technology of artificial amber preparation.
CLAIM
A composition for artificial amber comprising a solution of polyglycol male terminal terephthalate in an unsaturated monomer or oligomer and rosin, characterized in that it additionally contains succinic acid with the following component ratio, mass parts:
A solution of polyglycol male terminal terephthalate in an unsaturated monomer or oligomer 100
Rosin 25 - 100
Amber acid 1 - 7
2. A process for producing artificial amber by mixing a solution of polyglycolmaleinate phthalate in an unsaturated monomer or oligomer and rosin followed by curing, characterized in that additional succinic acid is added, the components of the composition are mixed and the mixture is solidified -radiation at a radiation dose of 8-20 Mrad at room temperature.
print version
Date of publication 02.01.2007гг
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