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INVENTION
Russian Federation Patent RU2171819
METHOD FOR PRODUCING COMPOSITE OF WATER GLUES
resorcin-formaldehyde resin
Name of applicant: JSC "Orgsintez"
Name of the inventor: Shmurak I.L .; Mitropolskaya RN .; Balabanov AI .; Usoltsev B.E .; VP Sobolev .; Anokhina EN
The name of the patentee: JSC "Orgsintez"
Address for correspondence: 125413, Moscow, ul. Naval 68, kv.41, I.L.Shmuraku
Starting date of the patent: 2000.01.28
The invention relates to a method of producing resorcinol resins which may find use in various technical fields as a component of adhesives, such as an aqueous adhesive for fastening to the textile materials in the rubber vulcanization process used in the tire and rubber industry. It describes a method of producing resorcinol resin by polycondensation of resorcinol and formaldehyde in the environment of a monohydric alcohol and ethylene glycol, comprising a preliminary condensation at 40-45 ° C and further maintaining the reaction mixture at reflux temperature followed by the addition of aqueous sodium hydroxide solution to pH 7.5-8.5 . The method is characterized in that the monohydric alcohol is butanol, the preliminary condensation is performed at this temperature for 1.5-2.5 h, then the reaction mixture was heated to 50-55 ° C at a temperature elevation rate 1-2 ° C / min and kept at boiling temperature until a viscosity of 30-60 s as per viscosity BZ-246. When this method is reduced flammability. Expand the range of resorcinol resins. The resin is characterized by high adhesion, which provides a high bond strength of rubber with textile materials.
DESCRIPTION OF THE INVENTION
The invention relates to methods for producing polycondensation polymers, in particular to a method of producing resorcinol resins which may find use in the production of adhesives, cold and hot curing used in the manufacture of plywood, wood laminates, fiberglass, in the tire and rubber industry.
Resorcin-formaldehyde resin is the main component of an aqueous adhesive - impregnating latex composition used in the fixing textile materials to rubber during vulcanization.
One of the necessary conditions for achieving a high rubber strength due to the use of a textile cord resorcinol novolac resin which is soluble in water.
Water-soluble resorcinol resin used in impregnating latex compositions are typically prepared in two steps to the same type of equipment based on the total batch process flowsheet. The process of obtaining partially condensed novolac type resorcinol resin is carried out at a molar ratio of formaldehyde to resorcinol is less than unity.
Incoming feed to the reactor was stirred until complete dissolution of resorcinol, formalin and then fed. The temperature conditions of the process depends on the requirements of the finished resin. Heating was continued until a desired viscosity resinous products. After polycondensation reactor jacket serves to bring the cold water of the resulting resin to normal temperature.
To increase the stability of the resin is added thereto an appropriate amount of sodium hydroxide solution with adjusting pH of resin to a value above 7.0.
Externally, the resorcinol resin is a uniform dark brown liquid with a faint odor of resorcinol. They possess thermoplastic properties. In preparation for gluing them converted into thermosetting resin. For this part of the resorcinol resin is introduced a certain amount of hardener - formaldehyde.
Known industrial process for obtaining resorcin-formaldehyde resin SF-280, comprising condensing resorcinol mixture with a fraction of crude phenol oil shale industry, boiling at 270 - 305 o C, in the ratio 1: 1, with formaldehyde by heating in a medium of alcohols in the presence of an acid catalyst (Production method a water-soluble resorcinol resin SF-280. The technological production regulations. shale plant "Kiviõli"). In this method, the preliminary condensation is carried out at 60 o C for 4 - 5 hours in a single environment and dihydric alcohols in the presence of zinc acetate as a catalyst, followed by boiling the mixture for 15 - 25 min.
Known improved process for producing water-soluble resin rezortsinforomaldegidnoy SF-280 (Ed.'s Certificate. USSR N 895996, C 08 G 8/18, publ. 01.09.82). According to this method, first conduct preliminary condensation of resorcinol with a mixture of phenols shale fraction boiling at 270 - 305 o C, in a ratio of 1: 1, with formaldehyde, in a medium mono- and dihydric alcohols, at 40 - 44 o C in the presence of an acid catalyst compound selected from the group consisting of acetic acid, and phthalic acid, anthranilic, followed by condensation of the products obtained at boiling temperature. Next there is the step of neutralization of 15% aqueous sodium hydroxide to pH 7,9 - 8,5.
The closest to the claimed method of producing a resorcinol resin SF-282 (FR-12) comprising polycondensation of resorcinol and formaldehyde by heating in a medium of ethyl alcohol and ethylene glycol, followed by neutralization with aqueous sodium hydroxide (V.P.Kondratev, YG Doronin . Water-resistant adhesives in wood. M .: Forest industry, 1988, p. 97). Condensation resins mode SF-282 as follows: Incoming feed to the reactor was stirred until complete dissolution of resorcinol. The temperature was raised to 40 - 45 o C and the reaction mixture was stirred for 4 hours. After keeping under continuous stirring the mixture is heated to boiling (98 - 100 o C). Duration of condensation at 98 - 100 o C, depending on the viscosity of the resin is 10 - 20 min. Upon reaching a viscosity of 20 - 25 at the OT-1 viskozometru condensation process ends. The mixture is cooled with continuous stirring to 30 - 35 o C and introduced into a 20% solution of sodium hydroxide. The condensation is continued for 30 min. Ready-SF-282 resin should have a viscosity of 15 - 30 and a pH in the range 7.5 - 8, 5.
However, all the above methods of the prior art are a fire hazard due to the use of ethanol and result in a resin with high adhesive properties is insufficient.
The problem to be solved by the present invention is to improve a method for producing and expanding the range of resorcinol resin with valuable performance properties.
The technical result that can be obtained by the practice of the invention is expressed in reducing fire hazard in the manufacture of resorcinol resin by eliminating from the process fire hazardous organic solvent - ethanol and improving the adhesion properties of the resin that can achieve improved performance rubber bond strength with textile cord, especially polyester cord.
The task is solved a new method of producing resorcinol resin.
According to a new method for the polycondensation of resorcinol and formaldehyde is carried out in a medium of two alcohols - monohydric alcohol and dihydric butanol - ethylene glycol and includes the following steps:
37% formalin and resorcinol butanol is stirred until complete dissolution resorcinol;
ethylene glycol and water introduced;
the mixture is heated to 40 - 45 o C and maintained at this temperature for 1.5 - 2.5 hours;
The reaction mixture was heated to 50 - 55 o C with a temperature rise rate of 1 - 2 o C / min, after which the mixture is heated and the exotherm due to the boil;
the mixture is kept at boiling temperature until a viscosity of 30 - 60 by viscometer VZ-246;
the resulting resin was cooled to 25 - 30 o C, was added 40% aqueous sodium hydroxide to pH 7.5 - 8.5, followed by stirring for 25 - 35 min.
The essence of the claimed invention is illustrated by the following examples of particular embodiment.
EXAMPLE 1 (Prior Art)
Mix 100 g of resorcinol, 20 g of ethanol, 10 g of ethylene glycol and the mixture was stirred until complete dissolution of resorcinol. Inject 38 g of 37% formalin, the mixture was heated to 40 - 45 o C and kept at this temperature for 4 hours.
The temperature was then raised to 100 o C and kept at this temperature for 20 min.
The resulting resin was cooled to 30 - 35 o C and 9 g administered 20% aqueous sodium hydroxide solution.
An aqueous adhesive composition (g, based on dry matter): carboxyl-butadiene latex SKD-1c in accordance with GOST 11604-79 100, SF-282 resin (Example 1) 16.5, 6.6 formaldehyde, sodium hydroxide 1.24. The adhesive contains water in an amount such that the solids content in the adhesive equals (13,0 ± 0,5)%. and a 25% aqueous solution of ammonia at the rate of 4 ml of n and 1 liter of glue. Glue is applied to the cord 25A anid brand TU 6-06-0279-89, cord dried for 5 minutes at 125 - 135 o C and determine the strength of the bond with his rubber-based SKI-3 isoprene rubber for H- method according to GOST 23785.7-89 . The results are shown in the table.
Example 2 (invention)
Mix 25 g of butanol, 31 g of 37% formalin, 100 g of resorcinol and the mixture was stirred until complete dissolution of resorcinol. Administered by 13.5 g of ethylene glycol and water, the mixture was heated to 40 - 45 o C and is kept 2 hours at this temperature. The mixture was then heated to 50 - 55 o C temperature rise at a rate of 1,5 o C / min, after which there is an exothermic heating it up to 85 - 90 o C and the mixture begins to boil. Boiling is maintained until the viscosity of the mixture of 30 - 60 by viscometer VZ-246.
The resulting resin was cooled to 25 - 30 o C and 9 g administered 40% aqueous sodium hydroxide solution, followed by stirring for 30 minutes.
Characteristics of the resulting resorcinol resin:
- Volume solids (dry matter),% - not less than 66
- Viscosity by viscometer VZ-246 with a - 30 - 60
- pH - 7,5 - 8,5
- The solubility in distilled water at a ratio of 1:25 - Full
Using the obtained resin, an aqueous adhesive of Example 1 was applied on its cord 25A of Example 1 and determine its bond strength with the rubber. The results are shown in the table.
Example 3 (Prior Art)
With the use of the resin obtained in Example 1, an aqueous adhesive composition (g, based on dry substance): butadiennitrilamidny latex SUA TU-52 100 2294-072-05766741-97 resin 25, 6, formaldehyde, sodium hydroxide 0.3.
The adhesive contains water in an amount such that the solids content in the adhesive equals 15.0 ± 0.5%, and a 25% aqueous ammonia solution at 6 ml per 1 l of glue. Glue is applied to the polyester cord 14P construction IIIteks x 1 x 2 TU 6-12-31-93, the cord is dried for 5 minutes at 155-165 o C and determine the strength of the bond with his rubber-based isoprene rubber SKI-3 and H-method according to GOST 23785.7-89.
The results are shown in the table.
example 4
With the use of the resin obtained in Example 2, an aqueous adhesive of Example 3 is applied on its 14P cord of Example 3, the cord is dried and determine its bond strength with the rubber. The results are shown in the table.
These tables show the advantage properties of the adhesive resin of the invention before resin prototype, which has resulted in improved bond strength performance rubber with textile cord.
Improved adhesive properties resorcinol resin obtained by carrying out the condensation process in the new mode, namely through precondensation holding for 1.5 - 2.5 hours by heating the reaction mixture of step with a certain speed to boiling and keeping to a certain viscosity.
Thus, the only set of operations and process parameters provides valuable performance properties of the resulting resorcinol resin.
In addition, reduced flammability of the process that is the most important achievement during the huge capacity of production.
CLAIM
A method of producing resorcinol resin by polycondensation of resorcinol and formaldehyde in the environment of a monohydric alcohol and ethylene glycol, comprising a preliminary condensation at 40-45 o C, and further maintaining the reaction mixture at reflux temperature followed by the addition of aqueous sodium hydroxide solution to pH 7.5-8.5, characterized in that the monohydric alcohol is butanol, the preliminary condensation is performed at this temperature for 1.5-2.5 h, then the reaction mixture is heated to 50-55 o C at a temperature elevation rate 1-2 o C / min and kept at boiling temperature until a viscosity of 30-60 s as per viscosity B3-246.
print version
Publication date 21.11.2006gg
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