CN116023533A - Neodymium phosphonate solution and preparation method and application thereof - Google Patents
Neodymium phosphonate solution and preparation method and application thereof Download PDFInfo
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- VMLVLKLHQLWCOB-UHFFFAOYSA-H [Nd+3].[Nd+3].[O-]P([O-])=O.[O-]P([O-])=O.[O-]P([O-])=O Chemical compound [Nd+3].[Nd+3].[O-]P([O-])=O.[O-]P([O-])=O.[O-]P([O-])=O VMLVLKLHQLWCOB-UHFFFAOYSA-H 0.000 title claims abstract description 113
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims description 137
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 50
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 claims description 40
- 239000007864 aqueous solution Substances 0.000 claims description 33
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 claims description 25
- -1 2-ethylhexyl oxy groups Chemical group 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 239000008346 aqueous phase Substances 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 125000003545 alkoxy group Chemical group 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 8
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 claims description 8
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 8
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 150000007514 bases Chemical class 0.000 claims description 4
- 150000001924 cycloalkanes Chemical class 0.000 claims description 4
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 4
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 239000002685 polymerization catalyst Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 13
- 238000009776 industrial production Methods 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000012071 phase Substances 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 18
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical group [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 14
- 229910052779 Neodymium Inorganic materials 0.000 description 9
- ZLMKQJQJURXYLC-UHFFFAOYSA-N bis(2-ethylhexoxy)-oxophosphanium Chemical compound CCCCC(CC)CO[P+](=O)OCC(CC)CCCC ZLMKQJQJURXYLC-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003926 complexometric titration Methods 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- PQAOATBZHSOOHQ-UHFFFAOYSA-N 1-hexoxyphosphonoyloxyhexane Chemical compound CCCCCCOP(=O)OCCCCCC PQAOATBZHSOOHQ-UHFFFAOYSA-N 0.000 description 1
- 239000004808 2-ethylhexylester Substances 0.000 description 1
- 125000003229 2-methylhexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000005916 2-methylpentyl group Chemical group 0.000 description 1
- HZIUHEQKVCPTAJ-UHFFFAOYSA-N 3-(2-ethylhexoxyphosphonoyloxymethyl)heptane Chemical compound CCCCC(CC)COP(=O)OCC(CC)CCCC HZIUHEQKVCPTAJ-UHFFFAOYSA-N 0.000 description 1
- RPAHVZMBEOTVNE-UHFFFAOYSA-N CCCCC(CC)CO[PH2]=O Chemical compound CCCCC(CC)CO[PH2]=O RPAHVZMBEOTVNE-UHFFFAOYSA-N 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 150000001206 Neodymium Chemical class 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical class OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 241000863480 Vinca Species 0.000 description 1
- CDOMXXVCZQOOMT-UHFFFAOYSA-N [phenoxy(phenyl)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(C=1C=CC=CC=1)(=O)OC1=CC=CC=C1 CDOMXXVCZQOOMT-UHFFFAOYSA-N 0.000 description 1
- 230000002152 alkylating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- PLSFNSJUKGEOSL-UHFFFAOYSA-N dioctoxy(oxo)phosphanium Chemical compound CCCCCCCCO[P+](=O)OCCCCCCCC PLSFNSJUKGEOSL-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- CDXVUROVRIFQMV-UHFFFAOYSA-N oxo(diphenoxy)phosphanium Chemical compound C=1C=CC=CC=1O[P+](=O)OC1=CC=CC=C1 CDXVUROVRIFQMV-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000007966 viscous suspension Substances 0.000 description 1
Abstract
The invention relates to the field of preparation of neodymium phosphonate, and discloses a neodymium phosphonate solution, a preparation method and application thereof. The neodymium phosphonate solution is characterized in that the solution viscosity of the neodymium phosphonate solution is lower than 200 mPa.s when measured at the concentration of 0.1mol/L at 25 ℃, and the chloride ion content in the neodymium phosphonate solution is not higher than 10ug/g when the concentration of the neodymium phosphonate is 0.1 mol/L. The neodymium phosphonate solution has the advantages of low viscosity and low impurity content, can be conveniently applied to industrial production, and is particularly favorable for conveying and accurate metering.
Description
Technical Field
The invention relates to the field of preparation of neodymium phosphonate, in particular to a neodymium phosphonate solution and a preparation method and application thereof.
Background
Phosphonates have been used as extractants for extracting metallic elements from rare earths, after which it has been found by accident that neodymium phosphonates have activity for catalyzing the polymerization of conjugated dienes. Both the national science vinca institute and michelin corporation have conducted studies based on phosphonate neodymium catalytic conjugated dienes to give products with high cis-1, 4-structure content (> 97%), and found that phosphonate neodymium is catalytically active at very low alkylating reagent levels ([ Al ]/[ Nd ] = 5), while other neodymium salt systems are catalytically inactive at such low aluminium levels. This feature makes the catalyst relatively low cost, creating advantages for industrial applications.
Currently, there are two methods of preparation of neodymium phosphonate. One is a solid process, for example, CN1479753a describes that the solid neodymium phosphonate obtained by this process cannot be completely dissolved in solvents commonly used in industry (alkane, toluene, etc.), the obtained catalyst is in a viscous suspension, and this heterogeneous catalyst may lead to a low utilization efficiency of neodymium atoms, and on the other hand may cause difficult transportation and inaccurate metering, which makes industrial production difficult. The second is a solution method, but the solution viscosity is large due to the characteristic of neodymium phosphonate, and is usually 10000mpa·s or more. This makes it difficult to delaminate the oil and water phases during the synthesis process, and water in the oil phase is difficult to remove, thereby causing the neodymium phosphonate to contain a large amount of impurities, further affecting the subsequent use. In addition, the high viscosity also makes the neodymium phosphonate have particularly poor fluidity and jelly shape, so that the neodymium phosphonate is difficult to accurately measure in application and cannot be used in industrial production.
In order to solve the problem of high viscosity, CN103694378A is added with a viscosity regulator, such as one or more of di (2-ethylhexyl) phosphonate, 2-ethylhexyl phosphonate-2-ethylhexyl ester, methyl phosphonate dimethyl heptyl, tributyl phosphonate, triphenyl phosphonate, dioctyl phosphonate, diethyl phosphonate, diphenyl phosphonate, dimethyl phthalate, diethyl phthalate and dioctyl phthalate, into a phosphonate neodymium solution after the synthesis reaction is finished, wherein the molar ratio of the addition of the viscosity regulator to neodymium in the organic phosphonate neodymium is 0.25-3:1. The addition of the viscosity modifier can significantly reduce the viscosity of the final product, but cannot solve the problem of high impurity content caused by difficult delamination in the synthesis process.
CN103224517a adds butadiene and/or isoprene and alcohols such as ethanol, propanol, butanol, hexanol, etc. to the oil phase, and although the solution viscosity is improved, the introduced alcohols are also an impurity for the subsequent use in rare earth catalysts.
Disclosure of Invention
The invention aims to provide a neodymium phosphonate solution, a preparation method and application thereof.
In a first aspect of the invention, there is provided a neodymium phosphonate solution, wherein the neodymium phosphonate solution has a solution viscosity of less than 200 mPa-s, measured at a concentration of 0.1mol/L at 25 ℃, and wherein the chloride ion content of the neodymium phosphonate solution is not higher than 10ug/g at a neodymium phosphonate concentration of 0.1 mol/L.
Preferably, the neodymium phosphonate solution has a solution viscosity of less than 100 mPa.s, measured at a concentration of 0.1mol/L at 25 ℃.
Preferably, the chloride ion content of the neodymium phosphonate solution is not higher than 7ug/g when the concentration of neodymium phosphonate is 0.1 mol/L.
Preferably, the neodymium ion concentration of the phosphonate neodymium solution is 0.04-0.5mol/L, preferably 0.1-0.2mol/L.
Preferably, the solvent of the neodymium phosphonate solution is n-hexane.
According to a second aspect of the present invention, there is provided a method for preparing the above neodymium phosphonate solution, wherein the method comprises: and a step of contacting a neodymium chloride aqueous solution, an organic phosphonate, an organic solvent and an alkaline compound, wherein the molar ratio of the organic phosphonate to neodymium chloride in the neodymium chloride aqueous solution is 4-6:1, and the alkaline compound is used in an amount such that the pH value of an aqueous phase is less than or equal to 5.
Preferably, the contacting comprises: after the aqueous solution of neodymium chloride is subjected to the first contact with the organic phosphonate and the organic solvent, the first contact product is subjected to the second contact with the alkaline compound.
Preferably, the content of neodymium chloride in the neodymium chloride aqueous solution is 0.1-0.5 mol/L.
Preferably, the molar ratio of the organic phosphonate to neodymium chloride in the neodymium chloride aqueous solution is 4-5:1.
Preferably, the organic phosphonate is of the structure shown in formula (1), wherein R d1 、R d2 And R is d3 Each independently is hydrogen, hydroxy, C 1 -C 20 Alkyl or C of (2) 1 -C 20 Alkoxy, and R d1 、R d2 And R is d3 At least one of which is C 1 -C 20 Alkyl or C of (2) 1 -C 20 Is a group consisting of an alkoxy group,
preferably, in formula (1), R d1 Is hydroxy, R d2 And R is d3 Are all 2-ethylhexyloxy groups.
Preferably, in formula (1), R d1 Is hydroxy, R d2 And R is d3 All are 2-ethylhexyl groups.
Preferably, in formula (1), R d1 Is hydroxy, R d2 Is 2-ethylhexyl, R d3 Is 2-ethylhexyl oxy.
Preferably, the organic solvent is C 5 -C 10 Alkanes, C 5 -C 10 Cycloalkanes and C 6 -C 12 One or more of the aromatic hydrocarbons of (a); more preferably, the organic solvent is one or more of hexane, cyclohexane, heptane, pentane, isopentane, octane, methylcyclohexane, benzene, toluene, xylene, and cumene.
Preferably, the organic solvent is used in an amount such that the volume of the organic phase to the volume of the aqueous phase is 0.3-2:1.
Preferably, the alkaline compound is used in an amount such that the pH of the aqueous phase is from 4 to 5.
Preferably, the alkaline compound is used in the form of an aqueous solution, and the content of the alkaline compound in the aqueous solution of the alkaline compound is 0.1-5.0 mol/L; more preferably, the second contacting is performed by dropping the aqueous alkali compound solution into the first contact product; more preferably, the drop velocity is 2.0 to 20.0mL/min.
Preferably, the basic compound is one or more of hydroxide and ammonia.
Preferably, the second contact temperature is 30 to 80 ℃.
According to a third aspect of the invention, there is provided a neodymium phosphonate solution prepared by the preparation method of the invention.
Preferably, the neodymium phosphonate solution has a solution viscosity of less than 200 mPa.s as measured at a concentration of 0.1mol/L at 25 ℃ and a chloride ion content of not more than 10ug/g at a neodymium phosphonate concentration of 0.1 mol/L.
Preferably, the neodymium phosphonate solution has a solution viscosity of less than 100 mPa.s, measured at a concentration of 0.1mol/L at 25 ℃.
Preferably, the chloride ion content of the neodymium phosphonate solution is not higher than 7ug/g when the concentration of neodymium phosphonate is 0.1 mol/L.
Preferably, the concentration of the neodymium phosphonate solution is 0.04-0.5mol/L, preferably 0.1-0.2mol/L.
Preferably, the solvent of the neodymium phosphonate solution is n-hexane.
According to a fourth aspect of the present invention, there is provided the use of a neodymium phosphonate solution of the present invention or a neodymium phosphonate solution prepared by a method of preparing a neodymium phosphonate solution of the present invention in the preparation of an olefin polymerization catalyst.
The neodymium phosphonate solution has the advantages of low viscosity and low impurity content, can be conveniently applied to industrial production, and is particularly favorable for conveying and accurate metering.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In a first aspect of the invention, there is provided a neodymium phosphonate solution having a solution viscosity of less than 200 mPa-s as measured at a concentration of 0.1mol/L at 25 ℃ and a chloride ion content of not more than 10ug/g at a neodymium phosphonate concentration of 0.1 mol/L.
According to the present invention, preferably, the neodymium phosphonate solution has a solution viscosity of less than 100 mPa-s measured at a concentration of 0.1mol/L at 25 ℃; more preferably, the neodymium phosphonate solution has a solution viscosity of less than 90 mPa-s measured at a concentration of 0.1mol/L at 25 ℃; further preferably, the neodymium phosphonate solution has a solution viscosity of 40-90 mPa.s measured at 25℃at a concentration of 0.1 mol/L.
Specific values of the solution viscosity of the neodymium phosphonate solution measured at 25℃at a concentration of 0.1mol/L include, for example: 5 mPas, 10 mPas, 20 mPas, 30 mPas, 40 mPas, 42 mPas, 50 mPas, 60 mPas, 65 mPas, 70 mPas, 80 mPas, 87 mPas, 90 mPas, 100 mPas, 112 mPas, 130 mPas, 150 mPas, 173 mPas or 190 mPas.
According to the present invention, preferably, the chloride ion content in the neodymium phosphonate solution is not higher than 10ug/g at a neodymium phosphonate concentration of 0.1 mol/L; more preferably, the chloride ion content is not higher than 9ug/g at a phosphonate neodymium concentration of 0.1 mol/L; more preferably; the chloride ion content is not higher than 8ug/g when the concentration of the neodymium phosphonate is 0.1 mol/L; more preferably; the chloride ion content is not higher than 7ug/g when the concentration of the neodymium phosphonate is 0.1 mol/L; still more preferably, the chloride ion content is 5-7ug/g at a phosphonate neodymium concentration of 0.1 mol/L.
Specific values of the chloride ion content include, for example: 1ug/g, 2ug/g, 3ug/g, 4ug/g, 5ug/g, 6ug/g, 7ug/g, 8ug/g, 9ug/g, or 10ug/g.
Preferably, the neodymium ion concentration of the phosphonate neodymium solution is 0.04-0.5mol/L, preferably 0.1-0.4mol/L, more preferably 0.1-0.3mol/L, more preferably 0.1-0.2mol/L, and even more preferably 0.1-0.16mol/L.
In the present invention, as described later, the solution viscosity is measured at 25℃using a rotary viscometer; the chloride ion content is measured according to the molar method in GB/T15453-2008; the concentration of the neodymium phosphonate solution was determined by complexometric titration. These methods are described in the publications and will not be described in detail.
The solvent in the neodymium phosphonate solution is preferably a preparation solvent according to the invention, and can be C 5 -C 10 Alkanes, C 5 -C 10 Cycloalkanes and C 6 -C 12 Preferably one or more of hexane, cyclohexane, heptane, pentane, isopentane, octane, methylcyclohexane, benzene, toluene, xylene and cumene; n-hexane is particularly preferred.
According to a second aspect of the present invention, there is provided a method for preparing the above neodymium phosphonate solution, wherein the method comprises: and a step of contacting a neodymium chloride aqueous solution, an organic phosphonate, an organic solvent and an alkaline compound, wherein the molar ratio of the organic phosphonate to neodymium chloride in the neodymium chloride aqueous solution is 4-6:1, and the alkaline compound is used in an amount such that the pH value of an aqueous phase is less than or equal to 5.
According to the invention, the aqueous solution of neodymium chloride can be obtained by reacting neodymium oxide with hydrochloric acid, or can be obtained by adopting a mode of dissolving anhydrous neodymium chloride or neodymium chloride containing crystal water in water. The concentration of neodymium chloride is not particularly limited as long as the neodymium chloride is ensured to be completely dissolved. For example, the concentration of the aqueous solution of neodymium chloride may be 0.1 to 0.5mol/L. In actual operation, since neodymium oxide, anhydrous neodymium chloride or neodymium chloride containing crystallization water of some manufacturers contains a very small amount of substances insoluble in water, in order to ensure the quality of subsequent products, when the conditions are met, filter paper or stainless steel mesh is preferably adopted to filter the neodymium chloride aqueous solution for reuse.
According to the present invention, preferably, the molar ratio of the organic phosphonate to neodymium chloride in the neodymium chloride aqueous solution is 4 to 5:1. By making the molar ratio of the organophosphonate to neodymium chloride in the neodymium chloride aqueous solution within the above-described range, the activity for the catalyst can be further improved.
According to the present invention, preferably, the organic phosphonate is of the structure represented by formula (1), wherein R d1 、R d2 And R is d3 Each independently is hydrogen, hydroxy, C 1 -C 20 Alkyl or C of (2) 1 -C 20 Alkoxy, and R d1 、R d2 And R is d3 At least one of which is C 1 -C 20 Alkyl or C of (2) 1 -C 20 Alkoxy groups of (a); preferably R d1 、R d2 And R is d3 Each independently is hydroxy, C 4 -C 12 Alkyl or C of (2) 4 -C 12 Alkoxy, and R d1 、R d2 And R is d3 At least one of which is C 4 -C 12 Alkyl or C of (2) 4 -C 12 Alkoxy groups of (a); more preferably, R d1 Is hydroxy, R d2 And R is d3 At least one of which is alkyl or alkoxy, and R d2 And R is d3 Each independently selected from n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl, 2-methylpentyl, 2-ethylpentyl, n-hexyl, 2-methylhexyl, 2-ethylhexyl, n-heptyl, n-octyl, n-nonyl, n-decyl, n-undecyl, n-dodecyl, n-butoxy, isobutoxy, sec-butoxy, tert-butoxy, n-pentyloxy, 2-methylpentyloxy, 2-ethylpentyloxy, n-hexyloxy, 2-methylhexyloxy, 2-ethylhexyloxy, n-heptyloxy, n-octyloxy, n-nonyloxy, n-decyloxy, n-undecyloxy or n-dodecyloxy.
Specific examples of the organic phosphonate may be selected from, for example, one or more of the compounds shown in the following formulas:
in the formula (1), R d1 Is hydroxy, R d2 And R is d3 Are all 2-ethylhexyl oxy groups (namely, di (2-ethylhexyl) phosphonate);
in the formula (1), R d1 Is hydroxy, R d2 And R is d3 Are all 2-ethylhexyl (i.e., di (2-ethylhexyl) phosphinate);
in the formula (1), R d1 Is hydroxy, R d2 Is 2-ethylhexyl, R d3 Is 2-ethylhexyl oxy (namely, is (2-ethylhexyl) phosphoric acid mono-2-ethylhexyl ester).
The organic phosphonate compound according to the present invention may be obtained in a conventional manner in the art, for example, may be commercially available, or may be prepared by a conventional method in the art, and the present invention is not particularly limited thereto.
According to the invention, the organic solvent is a compound capable of dissolving neodymium organophosphonate, for example C 5 -C 10 Alkanes, C 5 -C 10 Cycloalkanes and C 6 -C 12 Preferably one or more of hexane, cyclohexane, heptane, pentane, isopentane, octane, methylcyclohexane, benzene, toluene, xylene and cumene.
The amount of the above-mentioned organic solvent is not particularly limited, and it is preferable that the amount of the organic solvent is such that the concentration of the final product is not higher than 0.5mol/L. Furthermore, the organic solvent is preferably used in such an amount that the volume of the organic phase to the volume of the aqueous phase is 0.3 to 2:1, more preferably 0.5 to 1:1.
According to the present invention, the above-mentioned contact may be performed by mixing an aqueous neodymium chloride solution, an organic phosphonate, an organic solvent and a basic compound together, or by mixing two or more kinds of the above-mentioned components and then mixing the above-mentioned components with each other. In order to provide the resulting neodymium phosphonate solution with a lower viscosity and lower impurity content, preferably, the contacting comprises: after the aqueous solution of neodymium chloride is subjected to the first contact with the organic phosphonate and the organic solvent, the first contact product is subjected to the second contact with the alkaline compound.
In the present invention, the first contact is for sufficiently dissolving the reaction raw material, and preferably, the temperature of the first contact may be, for example, 5 to 80 ℃, and from the viewpoint of energy saving, the first contact is preferably performed at 10 to 50 ℃. The time for the first contact is not particularly limited, and may be, for example, 1 minute or more, preferably 1 to 5 minutes, as long as the reaction raw materials can be dissolved well.
According to the invention, the alkaline compound is preferably used in such an amount that the pH of the aqueous phase is between 4 and 5.
According to the present invention, the alkaline compound is a substance having a pH of more than 7 by itself or after being formulated into an aqueous solution, preferably one or more of hydroxide and aqueous ammonia, more preferably one or more of sodium hydroxide, potassium hydroxide and aqueous ammonia. For the basic compound in solid form, it is usually formulated into an aqueous solution. The concentration of the aqueous solution is not particularly limited as long as sufficient dissolution is ensured, and may be, for example, 0.1 to 5.0mol/L.
Preferably, the aqueous alkaline substance solution is added dropwise, and the dropping speed may be 2.0 to 20.0mL/min, preferably 5.0 to 10.0mL/min, relative to 350mL of the material to be dropped. And if the dropping speed is too low, the production efficiency is too low, the dropping speed is too high, the product generation rate is high, and the layering and impurity separation of the final oil-water phase are not facilitated.
In the present invention, "the drop rate may be 2.0 to 20.0mL/min with respect to 350mL of the dropped material" means that the drop rate may be 2.0 to 20.0mL/min when the dropped material is 350mL, and the drop rate may be 4.0 to 40.0mL/min when the dropped material is 700mL, so as to determine the drop rate when the dropped material is different in volume.
According to the present invention, preferably, the second contact temperature is 30 to 80 ℃, more preferably 30 to 55 ℃, still more preferably 45 to 55 ℃, particularly preferably at 50 ℃, and both the reaction rate and the energy saving can be achieved by performing at 50 ℃.
The time for the second contact may be, for example, 1 hour or more, preferably 1 to 6 hours, and more preferably 1 to 2 hours, as long as the reaction is sufficiently performed.
According to a third aspect of the invention, there is provided a neodymium phosphonate solution prepared by the preparation method of the invention.
The solution viscosity of the neodymium phosphonate solution prepared by the preparation method is lower than 200 mPa.s at 25 ℃ when the concentration is 0.1mol/L, and the chloride ion content in the neodymium phosphonate solution is not higher than 10ug/g when the concentration of the neodymium phosphonate is 0.1 mol/L.
Preferably, the neodymium phosphonate solution has a solution viscosity of less than 100 mPa-s measured at a concentration of 0.1mol/L at 25 ℃; more preferably, the neodymium phosphonate solution has a solution viscosity of less than 90 mPa-s measured at a concentration of 0.1mol/L at 25 ℃; further preferably, the neodymium phosphonate solution has a solution viscosity of 40-90 mPa.s measured at 25℃at a concentration of 0.1 mol/L.
Preferably, the chloride ion content in the neodymium phosphonate solution is not higher than 10ug/g when the concentration of neodymium phosphonate is 0.1 mol/L; more preferably, the chloride ion content is not higher than 9ug/g at a phosphonate neodymium concentration of 0.1 mol/L; more preferably; the chloride ion content is not higher than 8ug/g when the concentration of the neodymium phosphonate is 0.1 mol/L; more preferably; the chloride ion content is not higher than 7ug/g when the concentration of the neodymium phosphonate is 0.1 mol/L; still more preferably, the chloride ion content is 5-7ug/g at a phosphonate neodymium concentration of 0.1 mol/L.
Preferably, the neodymium ion concentration of the phosphonate neodymium solution is 0.04-0.5mol/L, preferably 0.1-0.4mol/L, more preferably 0.1-0.3mol/L, more preferably 0.1-0.2mol/L, and even more preferably 0.1-0.16mol/L.
Preferably, the solvent of the neodymium phosphonate solution is n-hexane.
According to a fourth aspect of the present invention, there is provided the use of a neodymium phosphonate solution of the present invention or a neodymium phosphonate solution prepared by a method of preparing a neodymium phosphonate solution of the present invention in the preparation of an olefin polymerization catalyst.
The present invention will be described in detail by way of examples, but the present invention is not limited to the following examples.
In the following examples and comparative examples, the solution viscosity was measured at 25℃using a rotary viscometer, the chloride ion content was measured according to the molar method in GB/T15453-2008, and the neodymium ion concentration of the neodymium phosphonate solution was measured using a complexometric titration method.
Example 1
Into a 1000mL three-necked flask, 120mL of an aqueous solution of neodymium chloride having a concentration of 0.25mol/L, 200mL of n-hexane and 56g of di (2-ethylhexyl) phosphonate were charged, and the mixture was heated to 50℃in a water bath. Stirring was started, then an aqueous sodium hydroxide solution (0.50 mol/L) was added dropwise to the flask via a constant pressure funnel, and after 170ml was added dropwise (30 minutes elapsed), the reaction was continued for 30 minutes, and the pH of the aqueous phase was measured to be 4.0. Wherein the molar ratio of phosphonate to neodymium is 5.8. After the reaction is finished, standing and layering are carried out, oil-water phase layering is good, and the interface is free of turbid impurities. The oil phase was separated and the solution viscosity at 25℃was found to be 81 mPas, the chloride ion content in the solution was found to be 5.1ug/g and the concentration was found to be 0.148mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 3.4ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity was 42 mPas as measured at 25 ℃.
Example 2
Into a 1000mL three-necked flask, 120mL of an aqueous solution of neodymium chloride having a concentration of 0.25mol/L, 200mL of n-hexane and 48g of di (2-ethylhexyl) phosphonate were charged, and the mixture was heated to 50℃in a water bath. Stirring was started, then an aqueous sodium hydroxide solution of 0.50mol/L was added dropwise to the flask via a constant pressure funnel, and the reaction was continued for 30 minutes after 180ml was added dropwise (time-consuming 30 minutes), and the pH of the aqueous phase was measured to be 4.5. Wherein the molar ratio of phosphonate to neodymium is 5.0. After the reaction is finished, standing and layering are carried out, oil-water phase layering is good, and the interface is free of turbid impurities. The oil phase was separated and the solution viscosity at 25℃was found to be 131 mPas, the chloride ion content in the solution was found to be 6.4ug/g and the concentration was found to be 0.155mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 4.1ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity was 65 mPas as measured at 25 ℃.
Example 3
Into a 1000mL three-necked flask, 120mL of an aqueous solution of neodymium chloride having a concentration of 0.25mol/L, 250mL of n-hexane and 40g of di (2-ethylhexyl) phosphonate were charged, and the mixture was heated to 50℃in a water bath. Stirring was started, then, dropwise adding a sodium hydroxide aqueous solution having a concentration of 0.50mol/L to the flask via a constant pressure funnel was started, 190ml was added dropwise (40 minutes elapsed), the reaction was continued for 30 minutes, and the pH of the aqueous phase was measured to be 5.0. Wherein the molar ratio of phosphonate to neodymium is 4.1. After the reaction is finished, standing and layering are carried out, oil-water phase layering is good, and the interface is free of turbid impurities. The oil phase was separated and the solution viscosity at 25℃was found to be 118 mPas, the chloride ion content in the solution was found to be 6.2ug/g, and the concentration was found to be 0.118mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 5.3ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity was 87 mPa.s as measured at 25 ℃.
Example 4
Into a 1000mL three-necked flask, 120mL of an aqueous solution of neodymium chloride having a concentration of 0.25mol/L, 200mL of n-hexane and 40g of di (2-ethylhexyl) phosphonate were charged, and the mixture was heated to 50℃in a water bath. Stirring was started, then, dropwise adding a sodium hydroxide aqueous solution having a concentration of 0.50mol/L to the flask via a constant pressure funnel was started, 190ml was added dropwise (40 minutes elapsed), the reaction was continued for 30 minutes, and the pH of the aqueous phase was measured to be 5.0. Wherein the molar ratio of phosphonate to neodymium is 4.1. After the reaction is finished, standing and layering are carried out, oil-water phase layering is good, and the interface is free of turbid impurities. The oil phase was separated and found to have a solution viscosity of 198 mPas at 25℃and a chloride ion content of 7.4ug/g and a concentration of 0.151mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 4.9ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity was 112 mPa.s as measured at 25 ℃.
Example 5
Into a 1000mL three-necked flask, 120mL of an aqueous solution of neodymium chloride having a concentration of 0.25mol/L, 100mL of n-hexane and 52g of di (2-ethylhexyl) phosphonate were charged, and the mixture was heated to 50℃in a water bath. Stirring was started, then an aqueous sodium hydroxide solution (0.50 mol/L) was added dropwise to the flask via a constant pressure funnel, and the reaction was continued for 30 minutes after 170ml was added dropwise (40 minutes elapsed), and the pH of the aqueous phase was measured to be 4.0. Wherein the molar ratio of phosphonate to neodymium is 5.4. After the reaction is finished, standing and layering are carried out, oil-water phase layering is good, and the interface is free of turbid impurities. The oil phase was separated and the solution viscosity at 25℃was found to be 369 mPas, the chloride ion content in the solution was found to be 9.8ug/g and the concentration was found to be 0.292mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 3.4ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity measured at 25℃was 173 mPas.
Example 6
Into a 1000mL three-necked flask, 120mL of an aqueous solution of neodymium chloride having a concentration of 0.25mol/L, 200mL of n-hexane and 56g of di (n-hexyl) phosphonate were charged, and the mixture was heated to 50℃in a water bath. Stirring was started, then an aqueous sodium hydroxide solution (0.50 mol/L) was added dropwise to the flask via a constant pressure funnel, and after 170ml was added dropwise (30 minutes elapsed), the reaction was continued for 30 minutes, and the pH of the aqueous phase was measured to be 4.2. Wherein the molar ratio of phosphonate to neodymium is 5.5. After the reaction is finished, standing and layering are carried out, oil-water phase layering is good, and the interface is free of turbid impurities. The oil phase was separated and the solution viscosity at 25℃was 108 mPas, the chloride ion content in the solution was 7.2ug/g and the concentration was 0.141mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 5.1ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity was 66 mPas measured at 25 ℃.
Comparative example 1
Otherwise as in example 1, the amount of di (2-ethylhexyl) phosphonate was changed to 36g only, with a molar ratio of phosphonate to neodymium of 3.7. The pH of the aqueous phase was measured to be 3.5. After the reaction is finished, the oil-water phase is difficult to separate after standing, and a plurality of white unidentified substances are arranged on the interface. The oil phase was withdrawn, and the solution viscosity at 25℃was 12184 mPas, the chloride ion content in the solution was 35.7ug/g, and the concentration was 0.124mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 28.8ug/g.
The obtained neodymium phosphonate solution was diluted to 0.1mol/L with n-hexane, and the solution viscosity was 9840 mPas measured at 25 ℃.
Comparative example 2
The pH of the aqueous phase was measured to be 6.5 by changing the amount of the aqueous sodium hydroxide solution to 300mL in the same manner as in example 1. After the reaction is finished, the oil-water phase is very difficult to separate after standing, and obvious interfaces are basically difficult to observe. The oil phase was withdrawn, and the solution viscosity at 25℃was found to be 8908 mPas, the chloride ion content in the solution was found to be 67.2ug/g, and the concentration was found to be 0.082mol/L. When the concentration was 0.1mol/L, the chloride ion content in the solution was 82.0ug/g.
The obtained neodymium phosphonate solution was concentrated to 0.1mol/L, and the solution viscosity measured at 25℃was 11076 mPa.s.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. A neodymium phosphonate solution, characterized in that the neodymium phosphonate solution has a solution viscosity of less than 200 mPa-s, measured at a concentration of 0.1mol/L at 25 ℃, and the chloride ion content in the neodymium phosphonate solution is not higher than 10ug/g at a neodymium phosphonate concentration of 0.1 mol/L.
2. The neodymium phosphonate solution according to claim 1, wherein the neodymium phosphonate solution has a solution viscosity of less than 100 mPa-s measured at a concentration of 0.1mol/L at 25 ℃;
preferably, the chloride ion content of the neodymium phosphonate solution is not higher than 7ug/g when the concentration of neodymium phosphonate is 0.1 mol/L.
3. The neodymium phosphonate solution according to claim 1 or 2, wherein the concentration of the neodymium phosphonate solution is 0.04-0.5mol/L, preferably 0.1-0.2mol/L.
4. A neodymium phosphonate solution according to any one of claims 1-3, wherein the solvent of the neodymium phosphonate solution is n-hexane.
5. A method for preparing a neodymium phosphonate solution, comprising: and a step of contacting a neodymium chloride aqueous solution, an organic phosphonate, an organic solvent and an alkaline compound, wherein the molar ratio of the organic phosphonate to neodymium chloride in the neodymium chloride aqueous solution is 4-6:1, and the alkaline compound is used in an amount such that the pH value of an aqueous phase is less than or equal to 5.
6. The method of claim 5, wherein the contacting comprises: after the aqueous solution of neodymium chloride is subjected to first contact with organic phosphonate and organic solvent, the first contact product is subjected to second contact with alkaline compound;
preferably, the content of neodymium chloride in the neodymium chloride aqueous solution is 0.1-0.5 mol/L;
preferably, the molar ratio of the organic phosphonate to neodymium chloride in the neodymium chloride aqueous solution is 4-5:1;
preferably, the organic phosphonate is of the structure shown in formula (1), wherein R d1 、R d2 And R is d3 Each independently is hydrogen, hydroxy, C 1 -C 20 Alkyl or C of (2) 1 -C 20 Alkoxy, and R d1 、R d2 And R is d3 At least one of which is C 1 -C 20 Alkyl or C of (2) 1 -C 20 Is a group consisting of an alkoxy group,
preferably, in formula (1), R d1 Is hydroxy, R d2 And R is d3 All are 2-ethylhexyl oxy groups;
preferably, in formula (1), R d1 Is hydroxy, R d2 And R is d3 All are 2-ethylhexyl groups;
preferably, in formula (1), R d1 Is hydroxy, R d2 Is 2-ethylhexyl, R d3 Is 2-ethylhexyloxy;
preferably, the method comprises the steps of,the organic solvent is C 5 -C 10 Alkanes, C 5 -C 10 Cycloalkanes and C 6 -C 12 One or more of the aromatic hydrocarbons of (a);
preferably, the organic solvent is one or more of hexane, cyclohexane, heptane, pentane, isopentane, octane, methylcyclohexane, benzene, toluene, xylene, and cumene;
preferably, the organic solvent is used in an amount such that the volume of the organic phase to the volume of the aqueous phase is 0.3-2:1.
7. The method according to claim 5 or 6, wherein the alkaline compound is used in an amount such that the PH of the aqueous phase is 4 to 5;
preferably, the alkaline compound is used in the form of an aqueous solution, and the content of the alkaline compound in the aqueous solution of the alkaline compound is 0.1-5.0 mol/L; more preferably, the second contacting is performed by dropping the aqueous alkali compound solution into the first contact product; more preferably, the dropping speed is 2.0-20.0 mL/min;
preferably, the basic compound is one or more of hydroxide and ammonia.
8. The method of any one of claims 6 or 7, wherein the second contact temperature is 30-80 ℃.
9. A neodymium phosphonate solution prepared by the method for preparing a neodymium phosphonate solution according to any one of claims 5-8;
preferably, the neodymium phosphonate solution has a solution viscosity of less than 200 mPa.s as measured at a concentration of 0.1mol/L at 25 ℃ and a chloride ion content of not more than 10ug/g at a neodymium phosphonate concentration of 0.1 mol/L;
preferably, the neodymium phosphonate solution has a solution viscosity of less than 100 mPa-s measured at a concentration of 0.1mol/L at 25 ℃;
preferably, the chloride ion content in the neodymium phosphonate solution is not higher than 7ug/g when the concentration of neodymium phosphonate is 0.1 mol/L;
preferably, the concentration of the neodymium phosphonate solution is 0.04-0.5mol/L, preferably 0.1-0.2mol/L;
preferably, the solvent of the neodymium phosphonate solution is n-hexane.
10. Use of a neodymium phosphonate solution according to any one of claims 1 to 4 or a neodymium phosphonate solution according to any one of claims 5 to 8 in the preparation of an olefin polymerization catalyst.
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