Method of removing volatile impurities from epoxide resin and apparatus for implementation thereof
FIELD: polymer production.
SUBSTANCE: invention relates to removal of volatile impurities from epoxide resin used to manufacture of coatings. Method of invention resides in that container with epoxide resin is placed in tank with hot oil and heated to 100-110°C at stirring. When temperature of resin achieves 50°C, air is supplied to its lower layers.
EFFECT: increased degree of removing volatile impurities from epoxide resin and safety of process.
The invention relates to mechanical engineering and can be used to remove volatile impurities from the epoxy resin during its preparation for use in coatings products.
A known method of removing volatile impurities from epoxy resin (see Starostinski YU.N., The N. Mulyar. The shaping surfaces of solids of revolution epoxy computime. - M., 1989, p.20-21), (Machine-building production. A series of Progressive technological processes in machine-building. Overview of WNITER. N. 3)adopted for the prototype. The method consists in the fact that the epoxy resin was placed in a container, heated to a temperature of 50-60°With, mix the resin in the vessel and then endure the resin for 10-15 minutes.
The described method has the following disadvantages. Heating the resin to 50-60°does not allow to obtain a sufficient viscosity, affecting the rapid removal of volatile impurities. At this temperature the vapour pressure has a relatively small value, which is not conducive to intensive exchange of volatiles between the resin and air (mass transfer). Must be aged resin, which increases the duration of the process. Mixing of the resin does not provide the necessary mass transfer.
This method is carried out in known from the same information source device containing succinctly the th for resin, a device for heating the vessel and the stirrer placed inside the container.
This device for the reasons stated above in the description of the method does not provide high quality cleaning epoxy from volatile impurities. In addition, the device does not provide uniform heating of the epoxy resin and the maintenance of a constant heating temperature of the resin, which can lead to overheating and oxidation of the resin in the zone closest to its adhesion to the heating device and, therefore, reduce the quality of the obtained resin after removal of volatile impurities. The device does not provide a safe for humans removal of volatile impurities, because the evaporation of volatile substances occurs in the surrounding tank space.
This invention solves the problem of obtaining an epoxy resin with a high degree of purification from volatile impurities.
The present invention is directed to the achievement of the technical result consists in increasing the intensity and quality of purification of epoxy resin from volatile impurities, improving process safety.
To obtain the technical result in the proposed method of removal of volatile impurities from epoxy resin, comprising heating and mixing of the resin in the vessel, heating the resin is carried out until the temperature of 100-110°by placing the flask with the resin in the tank with the heated oil, upon reaching the temperature of the resin 50°in its lower layers give the air. Heating of the epoxy resin to a temperature of 100-110°allows to obtain the optimum viscosity of the resin, facilitating intensive treatment. Heating of the resin by placing the vessel in a tank of heated oil flows to produce heating of the epoxy resin, which improves the quality of the resin after removal of volatile impurities. The air in the lower layers of epoxy resin by heating the resin 50°allows to improve the mass transfer in the resin, which increases the intensity of the removal of volatile impurities and, consequently, improve the quality of cleaning of epoxy resin.
To obtain the technical result in the device for removing volatile impurities from the epoxy resin containing the capacity for resin, a device for heating the vessel and the stirrer placed inside the tank, a device for heating capacity made in the form of a tank filled with oil, which is placed inside the container, on the bottom of the tank under the installed capacity of the heating elements, and tanks installed drain valve, exhaust ventilation and piping for air supply, which is connected with the dispenser mounted on the bottom of the tank. The device is equipped with a control device and adjusting the heating temperature of the resin. The tank wall is made with heat is izoliruemye strips.
The device for heating the container in the form of a tank filled with oil, which is placed inside the tank and heating elements installed on the bottom of the tank under the tank, allows you to quickly and evenly conduct heat capacity through the heated oil, which eliminates the possibility of overheating of the resin in separate zones, which increases the quality epoxy resin after cleaning. Supply device pipeline and nozzle, through which the lower layers of epoxy resin supplied air increases the mass transfer of impurities between the resin and air and thereby helps to remove impurities not only from the surface "mirrors" poured into the container of epoxy resin, and also from the lower layers, which increases the intensity and quality of purification of epoxy resin from volatile impurities. Installed inside the tank drain valve allows you to drain the purified epoxy resin at the end of the process. Supply device exhaust ventilation allows you to remove volatile impurities, harmful to human health components, which increases process safety. The device is equipped with a control device and adjusting the heating temperature of the resin, which contributes to a qualitative process. The implementation of the walls of the tank with insulating strips at demi allows to reduce the energy consumption for heating of the epoxy resin.
The proposed method is implemented as follows. Epoxy resin is poured into the container, which is placed in a tank of heated oil. Produce heating of the resin with simultaneous stirring. When the temperature epoxy resin 50°in its lower layers give the air. Then continue to heat the epoxy resin to a temperature of 100-110°C. Heating of the epoxy resin to a temperature of less than 100°does not provide the level of viscosity, which is an intensive cleaning of the resin, and heating of the epoxy resin to a temperature above 110°leads to oxidation of the resin, deteriorating the water quality after treatment. In addition, at a temperature of 100-110°With the pressure of saturated vapors constituting a significant proportion of volatile impurities, approaching atmospheric. To increase the mass transfer in the lower layers of epoxy resin serving the air. The air bubbles up through the thickness of the resin saturated vapors of volatile impurities are removed from the resin. The combination of increased surface mass transfer and high vapor pressure impurities promotes mass transfer of volatile impurities, which prevents the maturation of epoxy resin. Thus the air begin to apply at the temperature of epoxy resin 50°because at lower temperatures the viscosity of the resin is still high and the air is not able to effectively participate in the mass transfer. agri capacity resin with the heated oil flows to produce heating of the epoxy resin and avoid overheating (oxidation resin), as there is no direct contact of the heating elements and capacity.
A device for removing volatile impurities from the epoxy resin has a reservoir 1 for resin, placed in tank 2 with oil. At the bottom of the tank 2 under the installed capacity of the heating elements 3. The tank 1 is equipped with a cover 4, in which is mounted exhaust ventilation 5 and the pipe 6 for supplying air into the lower layers of epoxy resin through a nozzle 7 mounted on the bottom of the tank 1. The device is equipped with a device 8 for control and adjustment of the heating temperature epoxy resin. The walls of the tank 2 is provided with insulating spacers 9. The device is equipped with a stirrer 10 is placed inside the container 1. It also has a discharge valve 11, one end of which is connected to the bottom part of tank 1.
Diagram of the device illustrated in the drawing.
The device operates as follows. Epoxy resin to be treated is poured through a nozzle in the lid 4 into the container 1 and is heated to a temperature of 50°With mixed resin mixer 10. Heating the vessel 1 passes through the oil heated by the heating elements 3. Through the pipe 6 and the nozzle 7 into the lower layers of the resin serves the air pressure of 0.4 MPA. Heating continues until the temperature of the resin 100-110°C. the Device 8 controls the heat and maintains the predetermined rate is the atmospheric temperature. The formed bubbles when passing through the heated resin combine with volatile impurities are removed in the exhaust ventilation 5. At the end of the cleaning process through the discharge valve 11 produce discharge of treated resin.
According to GOST 10587-84 "Tar epoxy uncured" 1.3 mass fraction of volatile impurities (epichlorohydrin, toluene, etc. in the resin ED-22 ED-20 ED-16, ED-6, the premium should not exceed 0.2%.
For a technical analysis of the used epoxy resin ED-20. Before cleaning resin produced the first measurement to determine the mass fraction of the volatile impurities. Method for the determination of volatile impurities in the epoxy resins described in GOST 22456-77. Determination of mass fraction of volatile impurities X1percentage is calculated by the formula (GOST 22456-77 3.2)
where m is the mass of the Cup, g;
m1- the mass of the Cup with the test material, g;
m2- the mass of the Cup dried test material, g;
Mass of Cup 23,9735;
The weight of the Cup with the test material 25,2354;
The weight of a Cup of dried material 25,2288,
Mass fraction of volatile impurities to the first measurement is equal to:
Then the resin filled in the installation, the pre-pogorelich 50° With over 9 minutes after turning the air flow produced the second measurement and the determined mass fraction of volatile impurities:
where 25,1213 g is the mass of the Cup with the test material;
25,1203 g mass of Cup of dried material.
After 12 minutes after turning the air flow produced the third measurement and the determined mass down volatiles:
where 25,1985 g is the mass of the Cup with the test material;
25,1984 g mass of Cup of dried material.
The data are summarized in table 1.
Thus, we can conclude that the removal efficiency of volatile impurities from epoxy resin made according to the proposed method is very high.
Method of removing volatile impurities from epoxy resin, comprising heating the epoxy resin to a temperature of 100-110°vessel under stirring, wherein the heating of the resin is carried out by placing the container with epoxy resin in a tank of heated oil, and when the temperature of the resin 50°in its lower layers give the air.
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to a method for preparing oxirane. Method involves interaction of olefin and peroxide compound in the presence of catalyst and solvent in at least two in-line fitted reactors and each reactor comprises part of catalyst. Method is carried out for two successive epoxidation reactions with intermediate distillation. Method provides reducing formation of by-side substances.
EFFECT: improved preparing method.
10 cl, 1 dwg, 2 ex
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to a method for preparing oxyrane. Method involves reaction of olefin with peroxide compound in the presence of catalyst and a solvent in at least two reactors arranged in series and each reactor contains part of catalyst. Peroxide compound is added to the first reactor only and the next or the following reactors are fed with peroxide compound presenting in medium preparing from the preceding reactor but not with fresh peroxide compound or used in this preceding reactor. Method provides enhancing output and reducing formation of by-side products.
EFFECT: improved method for preparing.
10 cl, 1 dwg, 2 ex
SUBSTANCE: film evaporator comprises vertical cylindrical housing, face lids, top and bottom tube plates, heat exchanging pipes, film generators mounted with a spaced relation inside the top ends of the heat exchanging pipes, and connecting pipes for supplying and discharging fluid that heat secondary steam and condensate. The bottom section of the housing receives pipeline made of a coil whose one end is connected with the connecting pipe for supplying the fluid and straight section is secured between the tube plates. The connecting pipe for supplying fluid is mounted in the bottom face lid of the evaporator and provided with two additional tube plates arranged under the top and bottom tube plates, respectively. The plates are provided with heat exchanging pipes and film generators arranged coaxially to the central axis of the housing. The device is provided with stiffening ribs that are arranged inside the housing and connect the adjacent pipes. The evaporator also has mechanism for axial movement of film generators. The film generators and heat exchanging pipes in the top section of the housing are provided with cones for adjusting the clearance for flowing fluid.
EFFECT: expanded functional capabilities.
1 cl, 9 dwg
FIELD: boiling-down crystallizing solutions; production of alumina.
SUBSTANCE: proposed method of boiling-down the aluminate solution is performed in evaporator working on natural circulation of solution at discharge of solution from heating (heat exchange) tubes to special chamber where injection of circulating solution is created similarly as in jet apparatus for increase of rate of its motion in heating tubes.
EFFECT: enhanced efficiency due to increased degree of circulation of solution through heating tubes at boiling of solution outside heating tubes.
FIELD: evaporation technique; chemical, nuclear, dairy, food-processing, wood-pulp and paper industries.
SUBSTANCE: proposed evaporator includes heating chamber with vertical heat exchange tubes arranged inside it and secured in tube sheets, separator, upper solvent chamber, unit for introducing and smoothly distributing the product to be evaporated which is made in form of film laid over heat exchange tubes; this unit is located in solvent chamber; evaporator is also provided with unit for introducing the vapor and product to separator, vapor inlet pipe union, branch pipe for discharge of separated product from separator, condensate and fixed gas outlet and inlet pipe unions. Upper tube sheets is divided into two parts by means of vertical partition; each part is provided with similar number of heat exchange tubes located in mirror image relative to vertical partition; first half of heat exchange tubes is connected with unit introducing and smoothly distributing the product to be evaporated which is made in form of film; lower ends of tubes located in mirror image are interconnected by means of passages. Unit for introducing the vapor and product into separator is made in form of separate branch pipes; one end of each said branch pipes is secured on upper end of respective heat exchange tube of second half of these tubes; other end is tangentially connected with separator.
EFFECT: extended functional capabilities due to evaporation of solution of foaming agents due to tangential delivery of product to be evaporated to evaporator divided into separate flows.