| PATENT NUMBER | This data is not available for free |
| PATENT GRANT DATE | April 2, 2002 |
| PATENT TITLE |
Product containing magnesium, halogen and alkoxy |
| PATENT ABSTRACT | The invention relates to a complex product containing magnesium, halogen and alkoxy, which has the following composition: Mg.sub.p X.sub.q (OR).sub.2p-q wherein X is a halogen, R is an alkyl group having from 1 to 20 carbon atoms, p is from 2 to 20 and q is from 1 to (2p-1). More specifically the complex product is a complex of the formula MgCl.sub.2.[Mg(OR).sub.2 ].sub.2 wherein R is an alkyl having from 4 to 10 carbon atoms. The complex is soluble in non-polar solvents and can be used in the preparation of transition metal components of Ziegler-Natta catalyst systems |
| PATENT INVENTORS | This data is not available for free |
| PATENT ASSIGNEE | This data is not available for free |
| PATENT FILE DATE | June 23, 2000 |
| PATENT CT FILE DATE | December 21, 1998 |
| PATENT CT NUMBER | This data is not available for free |
| PATENT CT PUB NUMBER | This data is not available for free |
| PATENT CT PUB DATE | July 8, 1999 |
| PATENT FOREIGN APPLICATION PRIORITY DATA | This data is not available for free |
| PATENT REFERENCES CITED |
Rompps Chemie-Lexikon, 7th Ed. Franckh'sche Verlagshandlung, W. Keller & Co., Stuttgart, 1973,Band 3, p. 1831. Principles of Organometallic Chemistry, Methuen & Co. London, 1971, pp. 60-61, Coates, G. E. et al. |
| PATENT PARENT CASE TEXT | This data is not available for free |
| PATENT CLAIMS |
What is claimed is: 1. A complex product containing magnesium, halogen and alkoxy, characterised in that it has the following formula (1): Mg.sub.p X.sub.q (OR).sub.2p-q (1) wherein X is a halogen, R is an alkyl group having from 1 to 20 carbon atoms, p is from 2 to 20, and 1.ltoreq.q 2. A complex product according to claim 1, characterised in that X is chlorine. 3. A complex product according to claim 1 or 2, wherein R is an alkyl group having from 1 to 16 carbon atoms. 4. A complex product according to claim 1, wherein p is from 3 to 20. 5. A complex product according to claim 3, wherein R is an alkyl group having 4 to 12 carbon atoms. 6. A complex product according to claim 1, wherein said complex product is soluble in a non-polar solvent. 7. A complex product according to claim 6, characterized in that it has the formula (4): MgCl.sub.2.[Mg(OR).sub.2 ].sub.2 wherein R is an alkyl group having 1-16 carbon atoms. 8. A complex product according to claim 1, wherein it shows an X-ray diffraction pattern having a halo between 14.degree. and 26.degree. 2.THETA.. 9. A process for the preparation of a complex product according to claim 1, containing magnesium, halogen and alkoxy, wherein a magnesium dihalide, an alcohol having from 1 to 20 carbon atoms, and a dialkyl magnesium having from 2 to 40 carbon atoms are reacted to form said complex product. 10. A process according to claim 9, characterised in that said magnesium dihalide is magnesium dichloride. 11. A process according to claim 9 or 10, wherein said alcohol is a compound of the formula ROH wherein R is an alkyl having 1 to 20 carbon atoms. 12. A process according to claim 9, wherein said dialkyl magnesium is a compound of the formula MgR'.sub.2, wherein each R' is the same or different and is an alkyl with 1 to 20 carbon atoms. 13. A process according to claim 9, comprising: a) reacting said magnesium dihalide and said alcohol to form an intermediate compound in liquid form, and b) reacting said intermediate compound in liquid form with said dialkyl magnesium to form said complex product. 14. A process according to claim 9, wherein said magnesium dihalide and said alcohol are reacted in a molar ratio of 1:2 to 1:8. 15. A process according to claim 9, said magnesium dihalide and said alcohol are reacted at 100 to 200.degree. C. 16. A process according to claim 9, wherein magnesium dihalide and said alcohol are reacted for 1 to 8 hours. 17. A process according to claim 13, wherein a solvent is added to keep said intermediate in liquid form. 18. A process according to claim 17, wherein said magnesium dihalide and said solvent are used in a molar ratio of 1:4 to 1:100. 19. A process according to claim 9, wherein said magnesium dihalide and said dialkyl magnesium are used in a molar ratio of 1:1 to 1:4. 20. A process according to claim 9, wherein said dialkyl magnesium is provided in the form of a hydrocarbon solution having a molar ratio between said dialkyl magnesium and the hydrocarbon of said solution of 1:2 to 1:10. 21. A process according to claim 20, wherein the hydrocarbon of said hydrocarbon solution is a hydrocarbon having 5 to 12 carbon atoms. 22. A process according to claim 9, wherein said complex product is recovered in the form of a solution. 23. A method for preparing an olefin polymerization catalyst by contacting the complex according to claim 1 with titanium compound. 24. A complex product according to claim 3, wherein R is an alkyl group having 6 to 10 carbon atoms. 25. The method process according to claim 23, wherein said complex or a reaction product thereof, is in liquid form impregnated on a catalyst support. 26. The method according to claim 23, wherein said complex is in the form on an insoluble polymeric complex, acting as a Mg provider and catalyst support. 27. The method according to claim 23, wherein said catalyst support is an inert support. 28. The method according to claim 23, wherein said catalyst support is an inorganic inert support. 29. The method according to claim 28, wherein said inorganic inert support is selected from the group consisting of silica, alumina, a mixed oxide, and a mixture thereof. 30. The method according to claim 28, wherein said inorganic inert support is silica. 31. The process according to claim 21, wherein the hydrocarbon of said hydrocarbon solution is an aliphatic hydrocarbon having 6 to 10 carbon atoms. 32. The process according to claim 20, wherein said solution is a hydrocarbon solution having a molar ratio between said dialkyl magnesium and the hydrocarbon of said solution of 1:4 to 1:8. 33. The process according to claim 19, wherein the molar ratio between said magnesium dihalide and said dialkyl magnesium is 1:1 to 1:2. 34. The process according to claim 17, wherein said magnesium dihalide and said solvent are used in a molar ratio of 1:12 to 1:24. 35. The process according to claim 17, wherein said magnesium dihalide and said solvent are used in a molar ratio of 1:10 to 1:40. 36. The process according to claim 17, wherein said solvent is a hydrocarbon. 37. The process according to claim 17, wherein said solvent is an aromatic hydrocarbon. 38. The process according to claim 17, wherein said solvent is toluene. 39. The process according to claim 16, wherein said magnesium dihalide and said alcohol are reacted for 2 to 6 hours. 40. The process according to claim 15, wherein said magnesium dihalide and said alcohol are reacted at 110 to 150.degree. C. 41. The process according to claim 14, wherein said magnesium dihalide and said alcohol are reacted in a molar ratio of 1:3 to 1:5. 42. The process according to claim 14, wherein said magnesium dihalide and said alcohol are reacted in a molar ratio of 1:4. 43. The process according to claim 12, wherein each R' is the same or different and is an alkyl with 2 to 12 carbon atoms. 44. The process according to claim 12, wherein each R' is the same or different and is an alkyl with 4 to 10 carbon atoms. 45. The process according to claim 11, wherein R is an alkyl having 4 to 12 carbon atoms. 46. The process according to claim 11, wherein R is an alkyl having 6 to 10 carbon atoms. 47. The complex product according to claim 7, wherein R is an alkyl group having 4 to 12 carbons. 48. The complex product according to claim 7, wherein R is an alkyl group having 6 to 10 carbon atoms. 49. The complex product according to claim 6, wherein said complex product is soluble in a hydrocarbon. 50. The complex product according to claim 6, wherein said complex product is soluble in an aromatic hydrocarbon. 51. The complex product according to claim 6, wherein said complex product is soluble in toluene. 52. The complex product according to claim 4, wherein p is from 3 to 10. 53. The complex product according to claim 4, wherein p is from 3 to 6. 54. The complex product according to claim 4, wherein p is from 3 to 4. 55. The complex product according to claim 4, wherein p is 3. -------------------------------------------------------------------------------- |
| PATENT DESCRIPTION |
The invention relates to a complex product containing magnesium, halogen and alkoxy. The invention also relates to a process for the preparation and use of such a complex product. By a complex product is meant either a distinct complex or a mixture of complexes. To be able to activate magnesium with TiCl.sub.4 to produce amorphous MgCl.sub.2 for a Ziegler-Natta catalyst, the magnesium has to be brought in a reactive state with respect to TiCl.sub.4. This is commonly done in two ways: 1. By forming a complex between MgCl.sub.2 and an organic compound having an active hydrogen like an alcohol ROH. This MgCl.sub.2.mROH complex is allowed to react with TiCl.sub.4. Thereby amorphous MgCl.sub.2 * is liberated. Equivalent amounts of titanous waste material: TiCl.sub.3 OR and HCl are formed. This waste material has to be washed away with an excess of TiCl.sub.4, which is a disadvantage. 2. By forming a Mg-alcoholate, i.e. Mg(OR).sub.2. This reacts with TiCl.sub.4 to give amorphous MgCl.sub.2 *. An equivalent of waste material, TiCl.sub.3 OR, is formed also here. MgR.sub.2 is soluble in inert hydrocarbon and reacts with TiCl.sub.4 to give amorphous MgCl.sub.2 * but as MgR.sub.2 is a strong reduction agent, an equivalent proportion of TiCl.sub.3 is co-precipitated with the MgCl.sub.2 *. The co-precipitation of TiCl.sub.3 is a disadvantage when preparing a high yield polypropylene Ziegler-Natta catalyst. With Grignard reagents like RMgCl and RMgBr, a strong solvent, i.e. an ether is needed to keep them in solution. If this kind of reagent is reacted with TiCl.sub.4, amorphous MgCl.sub.2 * is formed but at the same time TiCl.sub.4 complexates with all the R--O--R-oxygen atoms of the ether and a large amount of a catalytically inactive by-product complex R.sub.2 O--TiCl.sub.4 is formed. The reagents, reacting with TiCl.sub.4 to give amorphous MgCl.sub.2 * are listed in Table 1. In Table 1, CH denotes hydrocarbon. TABLE A Reagents reacting with TiCl.sub.4 giving amorphous MgCl.sub.2 * Reagent MgCl.sub.2.ROH Mg(OR).sub.2 MgR.sub.2 ClMgR Solvent CH CH CH R--O--R Reaction by product HClTiCl.sub.3 OR TiCl.sub.3 OR TiCl.sub.3 R.sub.2 O--TiCl.sub.4 According to Coates, G. E., et al., Principles of Organometallic Chemistry, Methuen & Co Ltd, London, 1971, pages 60 and 61, this type of complexes are prepared in diethyl ether, whereby e.g. a dimeric etherate is formed as follows: ##STR1## In the equation Me is methyl, Et is ethyl and tert-Bu is tertiary butyl. The etherate is dimeric in both benzene and ether media. The book also mentions that ether-free tert-BuOMgBr is insoluble in hydrocarbons and is likely to be polymeric. Tert-BuOMgCl can be assumed to behave in the same way, i.e. a strong polar solvent like an ether is needed to keep the reaction product in solution. WO 92/16533 discloses a process for producing alkoxymagnesium halides in a single step by stoichoimetrically reacting magnesium alkyl activated magnesium with an equimolar mixture of an alkyl halogenide and an alcohol. However, in this process an additional equimolar amount of alcohol is added to the reaction media to bring the components into a liquid state in a inert hydrocarbon solution. The achieved solution is thus not RO.Mg.Cl but RO.Mg.Cl.ROH. This solution will in this way contain an equimolar amount of ROH that will react with TiCl.sub.4 forming TiCl.sub.3 OR and HCl in a typical catalyst synthesis where TiCl.sub.4 is one of the reaction components. The same situation can be seen in WO91/05608 where MgCl.sub.2 is dissolved in 3ROH to produced MgCl.sub.2.3ROH that in turn is brought into contact with Mg(OEt).sub.2 to give an adduct of MgCl.sub.2.Mg(OEt).sub.2.3ROH. 1.6ROH is then removed from this adduct by azeotropic evaporation with heptane to give a product of EtO.Mg.Cl.0.7ROH corresponding to the product described in WO92/16533. WO 91/05608 added toluene and two different alcohols to magnesium chloride and refluxed for a short time. Then, dialkyl magnesium was added and the mixture was further refluxed. A complex of a magnesium haloalkoxide and two alcohols was obtained. Due to the alcohols in the complex, it was not suitable for the activation of TiCl.sub.4, see above. U.S. Pat. No. 4,727,051 reacted MgCl.sub.2 -ROH complexes and obtained stoichiometric compositions without giving their chemical structure. When using dissolved magnesium compounds for the activation of the transition metal compound of a Ziegler-Natta procatalyst, such as magnesium chloride, MgCl.sub.2, dissolved in a polar solvent, or magnesium alkyl, MgR.sub.2 or RMgCl, dissolved in diethyl ether or a hydrocarbon, other problems arise. In the case of MgCl.sub.2, problems are caused by the large amount of polar solvent needed for dissolving MgCl.sub.2. Evaporation operations of the polar solvent during the process of procatalyst preparation are laborous and, besides, traces of polar solvent on the formed procatalyst has to be removed by separate chemical treatment. In the case of MgR.sub.2, if not reacted with TiCl.sub.4, a separate chlorination agent and a separate chlorination step is need for activation. In addition to this MgR.sub.2 and RMgCl have the drawback that they easily overreduce the transition metal and have to be modified to a less reductive form, e.g. to a magnesium alkoholate Mg(OR).sub.2, before use. When preparing the procatalyst from starting materials which will react into a final catalytically active complex, i.e. by means of a stoichiometric process, the product generally tends to have unsufficiently Mg and Cl (or other halogen) for satisfactory activity. Thus there is a need for starting materials having an enhanced amount of Mg and Cl (or other halogen) in their molecules. One purpose of the invention is to provide a soluble magnesium compound, which gives good activity and is soluble in non-polar solvents. The magnesium compound must not overreduce the transition metal, because overreduction leads to low procatalyst activity. Another independent purpose of the invention is to provide a molecule, which contains sufficiently Mg and Cl (or other halogen) to produce high catalytic activity when reacted stoichiometrically with other compounds into a procatalyst or a complete Ziegler-Natta catalyst system. The above problems have now been eliminated and the purposes fulfilled with a complex product containing magnesium, halogen and alkoxy, essentially characterised by having the following formula (1): Mg.sub.p X.sub.q (OR).sub.2p-q (1) wherein X is a halogen, preferably a chlorine, R is an alkyl group having from 1 to 20 carbon atoms, p is from 2 to 20 and q is The complex product according to the invention can, depending on the quality and quantity of elements and groups, be soluble in non-polar organic solvents. Thus, complexes which are both soluble and insoluble in non-polar solvents can be selected among the claimed complexes. The soluble complexes can e.g. be used as starting material for catalytically active stoichiometrical procatalyst complexes and the insoluble complexes can e.g. be used as supporting activators of the transition metal compounds. Further, the complex product of the invention is always less reductive than the above mentioned magnesium alkyls MgR.sub.2 and RMgX and is therefore more suitable for activation of the transition metal compound. The complex product has, even at its smallest Mg (p=2) and X (q=1) contents, more magnesium and halogen in its molecule unit than the above mentioned non-reductive Mg(OR).sub.2. Whereas Mg(OR).sub.2 has Mg:X:OR=1:0:2, the claimed complex has at least the ratio M:X:OR=2:1:3. The chemical structure of the claimed complex product is based on the bivalence and bridge-forming ability of magnesium. It is believed, without limiting the scope of the invention, that the chemical structure is (a): ##STR2## wherein each G is the same or different and is selected from said X and said OR to form q units of X and 2p-q units of OR, and p is from 3 to 20. If p/3 is greater than 1 there is in formula (a) a . . . --bridge from the furthest Mg--G to the nearest M--G of the next unit. The chemical structure can also be (b): ##STR3## wherein each G is the same or different and is selected from said X and said OR to form q units of X and 2p-q units of OR, and p is from 3 to 20, or (c): ##STR4## wherein each G is the same or different and is selected from said X and said OR to form q units of X and 2p-q units of OR, and p is from 3 to 20. Most probably the claimed complex product has the structure of an equilibrium between structures (a), (b) and (c), as illustrated by the following trimer equilibrium of a MgCl.sub.2.[Mg(OR).sub.2 ].sub.2 complex: ##STR5## In the above formulas (a.sub.1), (a.sub.2), (b) and (c), Cl can be replaced by any halogen such as fluorine, chlorine, bromine and iodine, but the purposes of the invention are best fulfilled with chlorine. The alkyl R of the alkoxy group can be any alkyl suitable for the purpose of the invention. Similar structure and solubility parameter to optional solvents give soluble complexes for stoichiometric preparation of active procatalyst complexes. Different structure and solubility parameters give insoluble complexes for use as activating support. When a solvent having 5-10 carbon atoms, such as toluene, is used, R is preferably an alkyl group having from 1 to 16 carbon atoms, more preferably from 4 to 12 carbon atoms, most preferably from 6 to 10 carbon atoms. In the above formulas (a.sub.1), (a.sub.2), (b) and (c), p is chosen depending on the complex product's purpose of use. A higher oligomer (p.gtoreq.5) is less soluble and is suitable as supporting reagent, whereas e.g. a di-, tri- or tetramer is more soluble and suitable for e.g. homogenous and stoichiometric procatalyst preparation. Generally, p is preferably from 2 or 3 to 20, more preferably from 2 or 3 to 10. For homogenous and stoichoimetric preparation, p is preferably from 2 or 3 to 6, more preferably from 2 or 3 to 4, and most preferably 3. The number of halogens in the molecule agglomerate of the complex product can vary very much. As was initially established, a large amount of chlorine leads to insolubility in non-polar solvents, whereas good activity requires a large amount of halogen. This means that the amount of halogen has to be balanced. According to one embodiment, q is from 2 to p, preferably 2 (when p is 3). According to a preferable embodiment of the invention, the formula and structure of the claimed complex product is such that it is soluble in a non-polar solvent, preferably in a hydrocarbon, more preferably in an aromatic hydrocarbon, most preferably in toluene. Above, the claimed complex product has been described by means of its formula, probable structure and solubility. It is also proper to describe it according to its empirical, i.e. analytical composition. The claimed complex product preferably has the following empirical (Mg=1) composition (2): MgX.sub.a (OR).sub.b (2) wherein X and R are the same as above, a is 0.4-1.2 and b is 0.8 to 1.6. According to Rompps Chemie-Lexikon, 7. Ed., Franckh'she Verlagshandlung, W. Keller & Co., Stuttgart, 1973, Band 3, page 1831, a complex is a "derived name for compounds of higher order, which compounds are formed from molecules--in contrast to the compounds of first order, in the formation of which atoms participate". According to one embodiment of the invention, the claimed complex product is e.g. formed from the molecules MgCl.sub.2 and Mg(OR).sub.2 or ROMgCl and Mg(OR).sub.2. For example, it is a complex having a composition corresponding to the following formula (3): [MgCl.sub.2 ].sub.q/2.[Mg(OR).sub.2 ].sub.p-q/2 (3) wherein R, p and q are the same as above. Most preferably q is 2, i.e. it has a composition corresponding to the formula (4): MgCl.sub.2.[Mg(OR).sub.2 ].sub.2 (4) wherein R is the same as above. An important characteristic and feature of the claimed complex product is that it shows a X-ray diffraction pattern having a halo between 14.degree. and 26.degree. 2.THETA., more specifically between 18.degree. and 22.degree. 2.THETA.. The halo formation observed in the pattern of MgCl.sub.2.[Mg(OR).sub.2 ].sub.2 separates this complex from Mg(OR).sub.2, MgCl.sub.2.2ROH, MgCl.sub.2. C.sub.6 H.sub.4 (COOR).sub.2 and (MgCl.sub.2).sub.2.TiCl.sub.4.C.sub.6 H.sub.4 (COOR).sub.2 (C.sub.6 H.sub.4 (COOR).sub.2 is a typical internal phthalate electron donor), which all have a sharp distinct peak between 5.degree. and 10.degree. 2.THETA., but no halo formation between 18.degree. and 22.degree. 2.THETA.. The invention also relates to a process for the preparation of a complex product containing magnesium, halogen and alkoxy. In the process a magnesium dihalide, an alcohol having from 1 to 20 carbon atoms and a dialkyl magnesium having from 2 to 40 carbon atoms are reacted to form said complex product. It is preferable in the claimed process, that said magnesium dihalide is magnesium dichloride. Preferably, said alcohol is a compound of the formula ROH wherein R is an alkyl having 1 to 16 carbon atoms, preferably 4 to 12 carbon atoms, most preferably 6 to 10 carbon atoms. Said dialkyl magnesium is a compound of the formula MgR'.sub.2, wherein each R' is the same or different and is an alkyl with 1 to 20 carbon atoms, preferably 2 to 12 carbon atoms, most preferably 4 to 10 carbon atoms. Said complex product is preferably a complex product according to the above description. The claimed preparation process preferably has two steps. The process comprises: a) reacting said magnesium dihalide and said alcohol into an intermediate in liquid form, b) reacting said intermediate in liquid form with said dialkyl magnesium into said complex. Without limiting the scope of protection, the process can be described by the following equation: MgCl.sub.2 +4ROH.fwdarw.MgCl.sub.2.4ROH MgCl.sub.2.4ROH+2MgR'.sub.2.fwdarw.MgCl.sub.2 [Mg(OR).sub.2 ].sub.2 +4R'H In step a) of the two-step process of the invention, said magnesium halide and said alcohol are preferably reacted in a molar ratio of 1:2 to 1:8, more preferably 1:3 to 1:5, most preferably about 1:4. The magnesium halide and the alcohol are preferably reacted at 100 to 200.degree. C., most preferably at 110 to 150.degree. C. The reaction time between the alcohol and the magnesium halide is preferably 1 to 8 h, most preferably for 2 to 6 h. According to one embodiment a solvent, preferably a hydrocarbon, more preferably an aromatic hydrocarbon, most preferably toluene, is added to keep said intermediate in liquid form. The amount of solvent is preferably such that said magnesium halide and said solvent are used in a molar ratio of 1:4-1:100, more preferably 1:10-1:40, most preferably 1:12-1:24. In step b) of the claimed process said magnesium halide and said dialkyl magnesium are preferably used in a molar ratio of 1:1 to 1:4, preferably about 1:2. It is advantageous, if said dialkyl magnesium is provided in the form of a solution, preferably a hydrocarbon solution, most preferably a hydrocarbon solution having a molar ratio between said dialkyl magnesium and the hydrocarbon of said solution of 1:2 to 1:10, preferably 1:4 to 1:8. The hydrogen of said hydrocarbon solution is preferably a hydrocarbon having 5 to 12 carbon atoms, most preferably an aliphatic or aromatic hydrocarbon having 6 to 10 carbon atoms. According to the product description above, the complex product is preferably soluble so that an active procatalyst complex can be prepared directly by reacting the starting materials with each other. This means, that in the claimed preparation process, said reaction product is recovered in the form of a solution in said solvent or solvents. According to the initially defined purpose of the invention, the claimed complex product is used for the preparation of an olefin polymerisation catalyst, preferably the transition metal component of an olefin polymerisation catalyst, most preferably the titanium component of an olefin polymerisation catalyst. Naturally, the invention also relates to such a use. More specifically, said complex product is reacted with a titanium compound and preferably with an electron donor compound into said titanium component of an olefin polymerisation catalyst. As was also initially stated, said complex or a reaction product thereof is according to one embodiment of the invention in liquid form and preferably impregnated on an organic or inorganic catalyst support, more preferably an inert support, even more preferably an inorganic inert support such as silica, alumina, a mixed oxide or mixture thereof, and most preferably silica. According to another embodiment of the invention, said complex is in the form of an insoluble polymeric complex, acting as Mg provider and catalyst support. Experimental In the following the invention is exemplified, wherein the following figures are referred to: FIG. 1 shows the principles for preparing a solution containing the claimed complex. FIG. 2 shows the X-ray diffraction patterns of Mg(OR).sub.2 (12.5 .ANG.) and for the MgCl.sub.2.2ROH (13.5 .ANG.). FIG. 3 shows most probable complexation of Mg(OR).sub.2 giving a 12.5 .ANG. distance between Mg. FIG. 4 shows the X-ray patterns of MgCl.sub.2.[Mg(OR).sub.2 ].sub.2 /C7H.sub.16 +toluene complexes--in top curve the ROH is 2-ethyl-hexanol, in bottom curve ROH is n-butyl alcohol. FIG. 5 shows comparison between X-ray diffraction patterns of silica and a pattern of the MgCl.sub.2.(Mg(OR).sub.2).sub.2. FIG. 6 shows resemblance of the reflecting distances in a complex MgCl.sub.2. Mg(OR).sub.2 compared to the construction of the Si--O--Si--O--Si silica material. FIG. 7 shows the principles of preparing complexes of the reference by blending mechanically MgCl.sub.2 and Mg(OR).sub.2. FIG. 8 shows the X-ray diffraction pattern for crystalline MgCl.sub.2. FIG. 9 shows the X-ray diffraction pattern for amorphous MgCl.sub.2. FIG. 10 shows the X-ray diffraction pattern for a mechanical blend of crystalline MgCl.sub.2 and Mg(OR).sub.2. FIG. 11 shows the X-ray diffraction pattern for a mechanical blend of amorphous MgCl.sub.2 and Mg(OR).sub.2. |
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