Method for preparing polyalkoxyalumoxanes, silica-free binding agent based on thereof

FIELD: chemistry of metalloorganic compounds, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing polyalkoxyalumoxanes of the general formula: RO{[-Al(OR)-O-]x[-Al(OR*)-O-]y}zH wherein z = 3-100; x + y = 1; R*/Al = 0.05-0.95; R means CnH2n+1; n = 1-4; R* means -C(CH3)=CHC(O)CnH2n+1; -C(CH3)=CHC(O)OCnH2n+1, and preparing a silica-free binding agent based on thereof for producing refractory corundum ceramics for precise casting by melting out models. Method is carried out by interaction of organoaluminum compound with alcohol and chelating agent in an organic solvent medium wherein compound of the general formula: AlL3 is used as organoaluminum compound wherein L means CnH2n+1, CnH2n+1O, (CnH2n+1)2AlO[(CnH2n+1)AlO]t wherein n = 1-4 and t = 2-10 that is subjected for interaction with water, alcohol and chelating agent at temperature 0-250°C wherein compound of the formula R*OH is used as a chelating agent wherein R* means -C(CH3)=CHC(O)CnH2n+1; -C(CH3)=CHC(O)CnH2n+1 in the mole ratio H2O : ROH : R*OH = p : x : y wherein p = 0.001-1; x = 0.05-0.95; y = 0.05-0.95, and x + y = 1. Also, invention describes a silica-free binding agent based on chelated polyalkoxyalumoxanes in the following ratio of components, wt.-%: chelated polyalkoxyalumoxane, 5-90, and aliphatic alcohol, the balance, up to 100. Invention provides preparing air-stable polyalkoxyalumoxanes and a silica-free binding agent based on thereof, simplifying technology in preparing the corundum composition suspension and fitness period of suspension is prolonged.

EFFECT: improved preparing method, improved and valuable properties of compounds.

3 cl, 3 tbl, 2 ex

 

The invention relates to methods for producing polyalkoxysiloxanes General formula:

where z=3÷100; x+y=1; R*/Al=0,05÷0,95; R=CnH2n+1; n=1÷4;

and getting on their basis beskriminalnoe binder for refractory corundum ceramics, in particular for ceramic forms accurate casting (LVM).

Creating beskriminalnoe binder corundum structure, not interacting with the poured metal at temperatures up to 1800°is promising for fabrication of ceramic shell molds LVM for precise geometrically-complex castings high alloy steels, super alloys and refractory metals, and refractory products that are in prolonged contact with the molten metal.

A method of obtaining a binder based hydrochloridw aluminum (U.S. Pat. RF 2102180, 22 1/16, 1998) for the manufacture of ceramic molds in foundries. According to this patent quality aluminium raw material use waste melting of aluminum alloys, which contain SiO2. As a result, the binder composition includes up to 20 wt.% SiO2that makes it impossible to use such a binder for ceramic forms LVM accurate geometrically-complex to pour the high-alloy steels, heat resistant super alloys and refractory metals.

The most promising class of compounds for creating beskriminalnoe binder corundum composition are polyalkoxysiloxanes in which aluminum atoms are linked by oxygen atoms.

Known closest to the proposed and adopted us as a prototype method to obtain polyorganosiloxanes interaction in the environment of an organic solvent at 25÷250°alyuminiiorganicheskikh compounds of the General formula R2Al[OAlR]nOAlR2where R is alkyl, n=0÷30, with monohydroxy alcohols or compounds containing acyloxy or amino group (Ed. The USSR 366207, 08 G 33/20, 1973).

However, these compounds and their solutions in organic solvents have low hydrolytic stability and exposure to the air instantly covered insoluble film, and then use them as a binder becomes impossible.

Known bestransheinyie binder (U.S. Pat. USA, 4216815, 164-518, 1980), under the brand names of Dispural and Catapal, based on water Zola monohydrate aluminum with a pH of 3.6÷4,4. They are used in the USA for the manufacture of corundum forms LVM for casting alloys containing highly reactive components, method of directional solidification. First synthesize higher trialkylaluminium, which is then oxidized, and arr is soumise the aluminum alkoxide hydrolyzing water, receiving colloidal solutions.

The disadvantages of a suspension prepared on such binders are: the necessity of wetting and antifoaming additives, narrow range pH environment that requires certain amounts of a mineral acid (such as HCl), a long preparation of suspension (for 24 hours)and low survivability.

The objective of this invention to provide a stable air polyalkoxysiloxanes, beskriminalnoe binder based on them, as well as the simplification of the preparation of suspensions corundum structure and increase its shelf life.

To solve this problem, a method for obtaining polyalkoxysiloxanes to create beskriminalnoe binding interaction alyuminiiorganicheskikh connection with alcohol and a chelating agent in the environment of an organic solvent, characterized in that as alyuminiiorganicheskikh connection charge connection General formula: AlL3where L - CnH2n+1WithnH2n+1O, (CnH2n+1)2AlO[(CnH2n+1)AlO]twhere n=1÷4, t=2÷10, which is subjected to interaction with 0÷250°With water, alcohol and a chelating agent, which take the compound of the formula R*OH, where R*=C(CH3SNA(O)nH2n+1; With(CH3)=SNC(O)OSnH2n+1; when mo is enom the ratio of N 2O:ROH:R*OH=p:x:y, where p=0.001÷1, x=0,05÷0.95, and y=0,95÷0,05, x+y=1.

Also proposed beskriminalnoe binder based aluminum compounds, characterized in that as the aluminum compounds it contains chelated polyalkoxyalkyl General formula: RO{[-Al(OR)-O-]x[-Al(OR*)-O-]y}zH, where z=3÷100; x+y=1; R*/Al of 0.05÷0,95; R=CnH2n+1; n=1÷4; R*=C(CH3)=CHC(O)nH2n+1; With(CH3)=SNC(O)OSnH2n+1and optionally an aliphatic alcohol, in the following ratio, wt.%:

chelated polyalkoxyalkyl5÷90
aliphatic alcoholthe rest is up to 100.

Solutions of chelated polyalkoxysiloxanes in organic solvents hydrolytically stable in air. To prepare beskriminalnoe binder, as solvents, it is preferable to use aliphatic alcohols, as the most accessible and least toxic.

Getting beskriminalnoe binder can be accomplished with the selection and analysis of chelated polyalkoxysiloxanes and its subsequent dissolution in an alcohol solvent or without allocation of chelated polyalkoxysiloxanes.

Getting the chelated polyalkoxy is Maksakov is as follows: in the atmosphere of inert gas (nitrogen, argon) under stirring to hydrocarbon (pentane, hexane, heptane, benzene, toluene and the like) the solution AlL3(or without solvent) at 0÷30°With added dropwise a specified number of chelating agent. Then the reaction mixture was kept under stirring for one hour at 30÷60°C, cooled to 10÷20°and add the specified amount of alcohol (specific humidity - H2O, wt.%) or mixture of alcohol and water. Next, the reaction mixture was kept under stirring until the cessation of gassing (L - CxH2x+1), and in the absence of outgassing (L - CxH2x+1O) at least 1 hour. The solvent is distilled off under atmospheric pressure and then under reduced pressure and a temperature of 100÷250°C. Cool to room temperature in a current of dry air or nitrogen take samples chelated polyalkoxysiloxanes analysis (NMR, IR spectra, Mn(cryoscopy), TGA and elemental analysis).

To obtain beskriminalnoe binder in chelated polyalkoxyalkyl dispense the estimated amount of the aliphatic alcohol, the reaction is stirred up to complete dissolution of chelated polyalkoxysiloxanes. Take samples for analysis (appearance, mass fraction % aluminum, the gelation time).

Chelated polyalkoxysiloxanes, depending on the x, y, z, R, R* in the compound (1)are either viscous liquids or solid glassy substance soluble in almost all organic solvents, slowly gidrolizuacy during prolonged storage in a humid atmosphere, reacting with acids and alkalis.

The chelated structure of polyalkoxysiloxanes proven by NMR27Al, IR-spectra, Mn(cryoscopy), TGA and elemental analysis.

In NMR spectra27Al signals detected atoms chetyrekhvalentnogo aluminum when 53,79 ppm, five-coordinated aluminum in ppm of 34.40, become six-coordinated aluminum in 0,81 ppm In IR-spectra of chelated polyalkoxysiloxanes observed absorption bands in the regions 610 cm-1(Al-O6), 780 cm-1(Al-O-Albridge), 850-900 cm-1, 980 cm-l(Al-O4), and 1070 1015 cm-1(Al-O-C), 1100, 1180, 1300 cm-1(C-O), 1535 cm-1(C=C), 1630 cm-1(C=O, connected by the coordination bond with atom Al), 2900, 2950 cm-1(C-H), 3500 cm-1(Al-OH).

The invention is illustrated by the following examples.

Example 1.

Apparatus equipped with a stirrer, thermometer, metering funnel, reflux condenser, inert fill gas and loads of 32.6 g polyisobutylene [-(ISO-C4H9)Al-O-]12(Mn=1347, Al=23,8 wt.%) and 130,4 g of toluene. With 10-30°add the 15.0 g of acetoacetic ester. Then the reaction mixture was kept under stirring for one hour at 60°C, cooled to 20°With temperature and added 10.8 g of ethyl alcohol (N2About to 0.05 wt.%). Next, the reaction mixture was kept under stirring until cessation of gas evolution, the solvent is distilled off under atmospheric pressure, and continuing the distillation of the solvent from the reaction mixture at 150°C for 1 hour at a residual pressure of 0.2÷0,4 kPa. After cooling to room temperature get to 37.2 g (yield 98,8 wt.%) chelated polyethoxysiloxane. In a stream of dry air or nitrogen take samples for analysis (NMR, IR spectra, Mn, TGA and elemental analysis).

Synthesized polyetilenetereftalate, elemental analysis found: 35,59; N 6,18; Al 20,54 wt.%; for C45H85O35Al12calculated: 35,79; N 5,63; Al 21,47 wt.%), Mn=1509; Mn(cryoscopy)=1500, TGA: Al2About340,86 wt.% (Al - 21,63 wt.%).

To obtain beskriminalnoe binder to 37,0 g polietilentereftalatnoy at a temperature of 25°add 63,0 g of ethanol, stirred the reaction mass to dissolve chelated polyethoxysiloxane. The content of Al - 8.0 wt.%, the gelation time is 30 hours. Unload the finished binder in glass or polyethylene containers.

Example 2.

In the apparatus, SN is Bunny stirrer, thermometer, metering funnel, reflux condenser, filled with inert gas (nitrogen, argon), download 50 g (ISO-C4H9)3Al under stirring at 0÷10°add 13,13 g of acetoacetic ester. Then the reaction mixture was kept under stirring for one hour at 50°C, cooled to room temperature and add 105,61 g of isopropyl alcohol and of 3.64 g of distilled water. Next, the reaction mixture was kept under stirring until cessation of gas evolution at a temperature of 50°C and cooled down to room temperature in a stream of dry air or nitrogen. Get 128,4 g beskriminalnoe binder (yield of 99.5 wt.%). The Al content is from 5.29 wt.%, the gelation time of 50 hours. Unload the finished binder in glass or polyethylene containers.

Other samples performed similarly to examples 1 or 2, the data shown in table 1.

The results of stability studies of the composition and properties beskriminalnoe binders on the basis of chelated polyalkoxysiloxanes during storage are shown in tables 2 and 3.

From table 2 it follows that when stored in a closed container, with periodic use of a portion of the binder to various studies, composition and properties beskriminalnoe binder for six months did not change. In addition, in airtight containers within five IU azev continued vitality corundum suspension, obtained on the basis of this binding (table 3).

Application beskriminalnoe binders on the basis of chelated polyalkoxysiloxanes does not require significant changes to the traditional technology of making shell molds using as a binder hydrolyzed solutions ethylsilicate.

Testing of mechanical properties of samples of shell molds made of suspension proposed binder, showed that beskriminalnoe binder on the basis of chelated polyalkoxysiloxanes allows to obtain membranes with bending strength after calcination at 900° - 5,0÷9,0 MPa, and at 1250°C - 14÷20 MPa, which provides the form in its casting installations directional crystallization (TC) and high-speed directional crystallization (MIC).

For equiax casting you can use the combined form as one or two of the surface layer form of corundum suspension on the basis beskriminalnoe binder guarantee accurate reproduction of the surface microrelief and configuration model and create a chemically inert barrier layer, which prevents the interaction of the melt with shell form.

Thus, the use of ready beskriminalnoe binders on the basis of chelated polyalkoxysiloxanes allows the create effective and reliable technological process of manufacturing of casting molds for high-alloy steels, heat-resistant alloys, titanium, etc.

TABLE 2

Changes in the composition (the content of Al2About3, wt.%) and properties beskriminalnoe binder during storage
Shelf life, months123456
№ № Index
1Al2About3, wt.%13,713,713,713,713,713,7
η, CST9,49,49,459,439,439,4
2Al2About3, wt.%10,410,410,410,410,410,4
η, CST6,76,66,696,76,696,7
3Al2About3, wt.%10,810,810,810,810,8
η, CST6,89to 6.886,896,9to 6.886,9
TABLE 3

Changing the binding properties beskriminalnoe binder during storage.
Description1st month6th month
Viscosity of the suspension when applying 1 and layer 2, s4042
Viscosity of the suspension when applying 3-7 layers, sec2828
The ultimate strength in static bending ' green ' shell samples, MPa4,2-4,84,4-5,1

1. The method of producing polyalkoxysiloxanes General formula (1):

where z=3÷100; x+y=1; R*/Al=0,05÷0,95; R=CnH2n+1; n=1÷4;

R*=C(CH3)=SNC(O)nH2n+1; With(CH3)=SNC(O)OSnH2n+1to create beskriminalnoe binding interaction of aluminiumand the ski connection with alcohol and a chelating agent in the environment of an organic solvent, characterized in that as alyuminiiorganicheskikh connection charge connection General formula: AlL3where L - CnH2n+1CnH2n+1O, (CnH2n+1)2AlO[(CnH2n+1)AlO]twhere n=1÷4, t=2÷10, which is subjected to interaction with 0÷250°With water, alcohol and a chelating agent, which take the compound of the formula R*OH, where R*=C(CH3)=SNC(O)nH2n+1; C(CH3)=CHC(O)OCnH2n+1; when the molar ratio of H2O:ROH:R*OH=p:x:y, where p=0.001÷1, x=0,05÷0.95, and y=0,95÷0,05, x+y=1.

2. Beskriminalnoe binder based aluminum compounds, characterized in that as the aluminum compounds it contains chelated polyalkoxyalkyl General formula:

RO{[-Al(OR)-O-]x[-Al(OR*)-O-]y}zH,

where z=3÷100; x+y=1; R*/Al=from 0.05 to 0.95; R=CnH2n+1; n=1÷4;

R*=C(CH3)=SNC(O)nH2n+1; With(CH3)=SNC(O)OSnH2n+1,

and optionally an aliphatic alcohol, in the following ratio, wt.%:

Chelated polyalkoxyalkyl5÷90
Aliphatic alcoholThe rest is up to 100



 

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