CN106243146A - Two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds and preparation method thereof - Google Patents
Two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds and preparation method thereof Download PDFInfo
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- CN106243146A CN106243146A CN201610602379.2A CN201610602379A CN106243146A CN 106243146 A CN106243146 A CN 106243146A CN 201610602379 A CN201610602379 A CN 201610602379A CN 106243146 A CN106243146 A CN 106243146A
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- oleic acid
- temperature
- ethyl tin
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- -1 oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds Chemical class 0.000 title claims abstract description 70
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 title claims abstract description 62
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000005642 Oleic acid Substances 0.000 title claims abstract description 62
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims description 62
- 238000006243 chemical reaction Methods 0.000 claims abstract description 56
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 37
- 150000002148 esters Chemical class 0.000 claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 14
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 7
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 56
- AHNBSGYALSWVOQ-UHFFFAOYSA-N COC(=O)[Sn](CC(Cl)Cl)C(=O)OC Chemical compound COC(=O)[Sn](CC(Cl)Cl)C(=O)OC AHNBSGYALSWVOQ-UHFFFAOYSA-N 0.000 claims description 49
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 42
- 239000003054 catalyst Substances 0.000 claims description 36
- 239000011521 glass Substances 0.000 claims description 36
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 31
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- 230000006837 decompression Effects 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 22
- CGOSCPFIHGMPHN-UHFFFAOYSA-N COC(=O)[Sn](CC)C(=O)OC Chemical compound COC(=O)[Sn](CC)C(=O)OC CGOSCPFIHGMPHN-UHFFFAOYSA-N 0.000 claims description 18
- 238000004821 distillation Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 17
- 230000032050 esterification Effects 0.000 claims description 16
- 238000005886 esterification reaction Methods 0.000 claims description 16
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 16
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 16
- 238000005660 chlorination reaction Methods 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 14
- 238000007664 blowing Methods 0.000 claims description 14
- 210000003298 dental enamel Anatomy 0.000 claims description 14
- 239000011265 semifinished product Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 13
- 208000035126 Facies Diseases 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 229910001868 water Inorganic materials 0.000 claims description 10
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical group Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000003456 ion exchange resin Substances 0.000 claims description 8
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 8
- GHKCSRZBNZQHKW-UHFFFAOYSA-N 1-sulfanylethanol Chemical class CC(O)S GHKCSRZBNZQHKW-UHFFFAOYSA-N 0.000 claims description 6
- ZCYZVNPFLTXYPE-KVVVOXFISA-N SC(C)O.C(CCCCCCC\C=C/CCCCCCCC)(=O)O Chemical class SC(C)O.C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZCYZVNPFLTXYPE-KVVVOXFISA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 235000013877 carbamide Nutrition 0.000 claims 5
- 238000010438 heat treatment Methods 0.000 claims 3
- 239000007788 liquid Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 125000004185 ester group Chemical group 0.000 abstract description 4
- 229920002521 macromolecule Polymers 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 6
- 239000005977 Ethylene Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 125000001475 halogen functional group Chemical group 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- NLOMWWAGCXLRQK-UHFFFAOYSA-N COC(=O)[Sn](CC)C(=O)OC.[Cl] Chemical compound COC(=O)[Sn](CC)C(=O)OC.[Cl] NLOMWWAGCXLRQK-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/22—Tin compounds
- C07F7/226—Compounds with one or more Sn-S linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a kind of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds, molecular formula is:
Description
Technical field:
The present invention relates to a kind of travel notes tin compound and preparation method thereof, more particularly, relate to a kind of two oleic acid sulfydryl second
Base alcohol ester dimethoxycarbonyl ethyl tin compound and preparation method thereof.
Background technology:
When halo ethylene resin and the compositions containing halo ethylene resin are converted to goods at present, it is by resin is heated
The mode thermoforming softened or melt forms product, namely powdered resin composition is transformed into melt substance, then
Required shape is obtained through extruded.Heat is produced by the friction occurred in compound in this course, softens halogen ethylene
Heat needed for resin combination is different with composition difference, but general between 165-210 DEG C.Halo ethylene resin is being higher than
To degrade under conditions of 100 DEG C, and degraded can cause halogen ethylene variable color and physical property to be lost, even can blackening become fragile down to not
Can use, in order to solve these problems, people have done multiple effort, as Chinese patent 93118446.0 disclose one organic
The patent of stannum stable compound and its preparation method and application, belongs to the heat stabilizer of halo ethylene resin, can suppress to colour in early days,
There is UV resistant and long-term thermal stability.But the cost that there is problems of product is high, raw material sources is not extensive, solves this
One problem has become urgent need.
Summary of the invention
An object of the present invention is to provide a kind of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds.
The two of the purpose of the present invention are to provide a kind of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
Preparation method.
The these and other objects of the present invention will be come to embody further by the following detailed description and explanation.
The two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention, molecular formula is:
The preparation method of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention, including walking as follows
Rapid:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. that will measure, concentrated hydrochloric acid and catalyst add in chlorination enamel reaction still, start stirring, while stir
Mixing limit and add glass putty, the mesh number of glass putty is: 400 mesh, is passed through dry hydrogen chloride gas simultaneously, and control reaction temperature is 50-85
DEG C, the solids after glass putty reacts completely, lowered the temperature, filter white, its composition is dichloro dimethoxycarbonyl ethyl stannum chemical combination
Thing intermediate, then the acrylic acid methyl ester. of excess residual is removed in the aqueous solution of urea washing by 0.5-4 mass %, refilters, does
Dry pure dichloro dimethoxycarbonyl ethyl tin compound intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 2 mercapto ethanol, oleic acid, catalyst adds in reaction kettle of the esterification, heats while stirring, when temperature is heated to 55-
When 70 DEG C, react 1-4 hour, obtain semi-finished product；Then it is again heated to 80-90 DEG C, under condition of negative pressure, controls this temperature and keep
Within 1-3 hour, obtain oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
The dichloro dimethoxycarbonyl ethyl tin compound intermediate that A, step B are prepared, oleic acid mercaptoethanol ester, ammonia,
Deionized water and catalyst add in synthesis reactor, control reaction temperature and are 60-70 DEG C, react 1-3 hour, then blowing, layering,
Organic facies carries out decompression distillation again, and what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.05-0.90MPa,
Response time: 3-4 hour, the final products then lower the temperature, filtered.
It is an option that the preparation side of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention
Method, comprises the steps:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. that will measure, concentrated hydrochloric acid and catalyst add in chlorination enamel reaction still, start stirring, while stir
Mixing limit and add glass putty, the mesh number of glass putty is: 400 mesh, is passed through dry hydrogen chloride gas simultaneously, and control reaction temperature is 50-85
DEG C, the solids after glass putty reacts completely, lowered the temperature, filter white, its composition is dichloro dimethoxycarbonyl ethyl stannum chemical combination
Thing intermediate, then the acrylic acid methyl ester. of excess residual is removed in the aqueous solution of urea washing by 0.5-2.5 mass %, refilter,
It is dried to obtain pure dichloro dimethoxycarbonyl ethyl tin compound intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 2 mercapto ethanol, oleic acid, catalyst adds in reaction kettle of the esterification, heats while stirring, when temperature is heated to 60-
When 75 DEG C, react 1.5-2.5 hour, obtain semi-finished product；Then it is again heated to 80-90 DEG C, under condition of negative pressure, controls this temperature
Keep 1.5-3 hour obtaining oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
The dichloro dimethoxycarbonyl ethyl tin compound intermediate that A, step B are prepared, oleic acid mercaptoethanol ester, ammonia,
Deionized water and catalyst add in synthesis reactor, control reaction temperature and are 60-65 DEG C, react 1.5 hours, then blowing, layering,
Organic facies carries out decompression distillation again, and what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.08-0.5MPa, instead
Between Ying Shi: 3-4 hour, the final products then lower the temperature, filtered.
The preparation method of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention, including walking as follows
Rapid:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. of 60-120 kilogram, the concentrated hydrochloric acid of 1-3 kilogram and 0.1-1.0 kg catalyst are added chlorination ward off
In porcelain reactor, starting stirring, add 50-80 kilogram of glass putty while stirring, the mesh number of glass putty is: 400 mesh, is passed through dry simultaneously
30-70 kilogram of hydrogen chloride gas, control reaction temperature be 50-85 DEG C, after glass putty reacts completely, lower the temperature, filter white
Solids, its composition is dichloro dimethoxycarbonyl ethyl tin compound intermediate, then by the urea water of 0.5-2.5 mass %
The acrylic acid methyl ester. of excess residual is removed in solution 20kg washing, refilters, is dried to obtain pure dichloro dimethoxycarbonyl ethyl stannum
Compound intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 40-60 kilogram of 2 mercapto ethanol, 160-200 kilogram of oleic acid, 2-5 kg catalyst adds in reaction kettle of the esterification,
Heat while stirring, when temperature is heated to 60-75 DEG C, reacts 1.5-2.5 hour, obtain semi-finished product；Then 80-it is again heated to
90 DEG C, under condition of negative pressure, control this temperature and keep 1.5-3 hour obtaining oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
The 80-120 kilogram of dichloro dimethoxycarbonyl ethyl tin compound intermediate that A, step B are prepared, 180-220 kilogram
Oleic acid mercaptoethanol ester, deionized water 80-120kg, the ammonia of content 10-20% 60-100 kilogram and 0.5 kg catalyst add
Entering in synthesis reactor, control reaction temperature and be 60-65 DEG C, react 1.5 hours, then blowing, layering, reduce pressure organic facies again
Distillation, what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.08-0.1MPa, the response time: 3-4 hour, so
Rear cooling, the final products of filtration.
It is preferred that the preparation method of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention,
Comprise the steps:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. of 80-100 kilogram, the concentrated hydrochloric acid of 1.5-2.5 kilogram and 0.5 kg catalyst are added chlorination ward off
In porcelain reactor, starting stirring, add 55-70 kilogram of glass putty while stirring, the mesh number of glass putty is: 400 mesh, is passed through dry simultaneously
44 kilograms of hydrogen chloride gas, control reaction temperature and be 50-85 DEG C, after glass putty reacts completely, lower the temperature, consolidating of filtering white
Body thing, its composition is dichloro dimethoxycarbonyl ethyl tin compound intermediate, then with the aqueous solution of urea of 0.5-2.5 mass %
The acrylic acid methyl ester. of excess residual is removed in 21kg washing, refilters, is dried to obtain pure dichloro dimethoxycarbonyl ethyl stannum chemical combination
Thing intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 45-55 kilogram of 2 mercapto ethanol, 170-190 kilogram of oleic acid, 3-4 kg catalyst adds in reaction kettle of the esterification,
Heat while stirring, when temperature is heated to 60-75 DEG C, reacts 1.5-2.5 hour, obtain semi-finished product；Then 80-it is again heated to
90 DEG C, under condition of negative pressure, control this temperature and keep 1.5-3 hour obtaining oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
The 90-100 kilogram of dichloro dimethoxycarbonyl ethyl tin compound intermediate that A, step B are prepared, 190-210 kilogram
Oleic acid mercaptoethanol ester, deionized water 100kg, the ammonia of content 10-20% 70-90 kilogram and 0.5 kg catalyst add conjunction
Become in still, control reaction temperature and be 60-65 DEG C, react 1.5 hours, then blowing, layering, organic facies is carried out decompression again and steams
Evaporating, what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.08-0.1MPa, the response time: 3-4 hour, then
Cooling, the final products filtered.
In the preparation method of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention, described
A diameter of DN100 of chlorination enamel reaction still, cylinder height: 4000mm, inside have hydrogen chloride gas body canal 3850mm, mixing speed
It is 450 revs/min, and has sampling observation panel, thermometer mouth and gauge port.
In the preparation method of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention, described
Catalyst is AlCl3、FeCl3, ion exchange resin: 732 types or 213 types.
It is preferred that the preparation method of the two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of the present invention,
Molecular formula is:
It is prepared as follows:
A, the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
By 92 kilograms of acrylic acid methyl ester .s, 2 kilograms of concentration is concentrated hydrochloric acid and the 0.5 kg catalyst AlCl of 31%3Add chlorine
Change in enamel reaction still, start stirring, add 60 kilograms of glass puttys while stirring, be passed through dry hydrogen chloride gas 37kg simultaneously,
This gas is passed through bottom reactor, and controlling reaction temperature is 60 DEG C, 3 hours response time, after glass putty reacts completely, and fall
Temperature, the solids that filters white, its composition is: dichloro dimethoxycarbonyl ethyl tin compound intermediate, then with 1% urine
The acrylic acid methyl ester. of element aqueous solution 20 kilograms washing excess residual, refilters, is dried to obtain pure dichloro dimethoxycarbonyl ethyl
Tin compound intermediate 132.1KG, yield is 95%.
B, the preparation of oleic acid mercaptoethanol ester:
By 50 kilograms of 2 mercapto ethanols (content: 99%, technical grade), 181 kilograms of oleic acid (content: 99%, technical grade),
3.5 kilograms of content be 93% concentrated sulphuric acid add in reaction kettle of the esterification, heat while stirring, when temperature is heated to 65 DEG C, instead
It is 2.2 hours between Ying Shi, obtains semi-finished product, be then again heated to 85 DEG C ,-0.096MPa under condition of negative pressure, control this temperature
Keeping 2 hours, then lower the temperature, filter to obtain oleic acid mercaptoethanol ester 215KG, yield is 98%.
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
By 100 kilograms of dichloro dimethoxycarbonyl ethyl tin compound intermediate, 206 kilograms of oleic acid mercaptoethanol esters, content
It is 80 kilograms of ammonia of 17%, 100 kilograms of deionized waters and ion exchange resin: 213 type catalyst add in synthesis reactor, control reaction
Temperature 65 DEG C, reacts 1.5 hours, then blowing, layering, by organic facies again carry out decompression distillation, decompression distillation control strip
Part is: temperature: 85-90 DEG C；Negative pressure :-0.098MPa；Response time: 3.5 hours, then lower the temperature, filter, obtain two oleic acid mercaptos
Base ethyl alcohol ester dimethoxycarbonyl ethyl tin compound 281KG, yield is 96.5%.
Technical solution of the present invention quotes oleic acid synthesis (inverse) Ester-tin Compounds, due to the change of (inverse) ester group structure,
The activity increase of (inverse) ester group so that it is as stabilizer early stage stability more preferably, then due in ester containing the oil of macromolecule
Acid so that it is slip is more excellent, has the effect that traditional organotin cannot possess.And use equipment and the technique of uniqueness, instead
Answer effect more preferable, in hgher efficiency, there is more preferable application prospect.
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
In the present invention, refering in particular to as non-, all of amount, part are unit of weight, and all of raw material all can be from market
Buy.
Detailed description of the invention
Embodiment 1
Prepare two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of following molecular formula:
It is prepared as follows:
A, the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
Sn+2CH2=CHCOOCH3+2HCL→(CH3COOCCH2CH2)2SnCL2
By 92 kilograms of acrylic acid methyl ester .s (content is: 99.0%, technical grade), 2 kilograms of concentration is the concentrated hydrochloric acid and 0.5 of 31%
Kg catalyst AlCl3Add in chlorination enamel reaction still, start stirring, add while stirring 60 kilograms of glass puttys (content is:
99.99%, technical grade, mesh number is: 400 mesh), it being passed through dry hydrogen chloride gas 37kg simultaneously, this gas is passed through Polycondensation Reactor and Esterification Reactor
Portion, in order to improve response speed, controlling reaction temperature is 60 DEG C, 3 hours response time, (sampling after glass putty reacts completely
Observing response situation), the solids lowered the temperature, filter white, its composition is: in the middle of dichloro dimethoxycarbonyl ethyl tin compound
Body, then the aqueous solution of urea 20 kilograms with 1% washs the acrylic acid methyl ester. of excess residual, refilters, is dried to obtain pure two
Chlorine dimethoxycarbonyl ethyl tin compound intermediate 132.1KG, yield is 95%；
B, the preparation of oleic acid mercaptoethanol ester:
HOCH2CH2SH+CH3(CH2) 7CH=CH (CH2)7COOH→
HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+H20
By 50 kilograms of 2 mercapto ethanols (content: 99%, technical grade), 181 kilograms of oleic acid (content: 99%, technical grade),
3.5 kilograms of content be 93% concentrated sulphuric acid add in reaction kettle of the esterification, heat while stirring, when temperature is heated to 65 DEG C, instead
It is 2.2 hours between Ying Shi, obtains semi-finished product, be then again heated to 85 DEG C ,-0.096MPa under condition of negative pressure, control this temperature
Keeping 2 hours, then lower the temperature, filter to obtain oleic acid mercaptoethanol ester 215KG, yield is 98%.
C, the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
(CH3COOCCH2CH2)2SnCL2+2HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+2NH3.H2O→
By 100 kilograms of dichloro dimethoxycarbonyl ethyl tin compound intermediate, 206 kilograms of oleic acid mercaptoethanol esters, content
It is 80 kilograms of ammonia of 17%, 100 kilograms of deionized waters and 0.5 kilogram of ion exchange resin: 213 type catalyst add in synthesis reactor,
Control reaction temperature 65 DEG C, react 1.5 hours, then blowing, layering, organic facies is carried out decompression distillation again, decompression distillation
Control condition be: temperature: 85-90 DEG C；Negative pressure :-0.098MPa；Response time: 3.5 hours, then lower the temperature, filter, obtain
Two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compound 281KG, yield is 96.5%.
Embodiment 2
Prepare two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of following molecular formula:
It is prepared as follows:
A, the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
Sn+2CH2=CHCOOCH3+2HCL→(CH3COOCCH2CH2)2SnCL2
By 65 kilograms of acrylic acid methyl ester .s (content is: 99.0%, technical grade), 1 kilogram of concentration is the concentrated hydrochloric acid and 0.3 of 31%
Kg catalyst AlCl3Add in chlorination enamel reaction still, start stirring, add while stirring 50 kilograms of glass puttys (content is:
99.99%, technical grade, mesh number is: 400 mesh), it being passed through dry hydrogen chloride gas 30kg simultaneously, this gas is passed through Polycondensation Reactor and Esterification Reactor
Portion, in order to improve response speed, controlling reaction temperature is 50 DEG C, in 2.5 hours response time, (takes after glass putty reacts completely
Sample observing response situation), the solids lowered the temperature, filter white, its composition is: in dichloro dimethoxycarbonyl ethyl tin compound
Mesosome, then the aqueous solution of urea 20 kilograms with 1% washs the acrylic acid methyl ester. of excess residual, refilters, is dried pure
Dichloro dimethoxycarbonyl ethyl tin compound intermediate 102.1KG, yield is 94%；
B, the preparation of oleic acid mercaptoethanol ester:
HOCH2CH2SH+CH3(CH2) 7CH=CH (CH2)7COOH→
HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+H20
By 40 kilograms of 2 mercapto ethanols (content: 99%, technical grade), 161 kilograms of oleic acid (content: 99%, technical grade),
2.5 kilograms of content be 93% concentrated sulphuric acid add in reaction kettle of the esterification, heat while stirring, when temperature is heated to 65 DEG C, instead
It is 1.6 hours between Ying Shi, obtains semi-finished product, be then again heated to 82 DEG C ,-0.096MPa under condition of negative pressure, control this temperature
Keeping 2 hours, then lower the temperature, filter to obtain oleic acid mercaptoethanol ester 185KG, yield is 98%.
C, the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
(CH3COOCCH2CH2)2SnCL2+2HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+2NH3.H2O→
By 80 kilograms of dichloro dimethoxycarbonyl ethyl tin compound intermediate, 186 kilograms of oleic acid mercaptoethanol esters, content is
60 kilograms of ammonia of 17%, 80 kilograms of deionized waters and 0.3 kilogram of ion exchange resin: 213 type catalyst add in synthesis reactor, control
Reaction temperature 65 DEG C, reacts 1.5 hours, then blowing, layering, by organic facies again carry out decompression distillation, decompression distillation control
Condition processed is: temperature: 85-90 DEG C；Negative pressure :-0.098MPa；Response time: 3.5 hours, then lower the temperature, filter, obtain two oil
Acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compound 201KG, yield is 96.5%.
Embodiment 3
Prepare two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of following molecular formula:
It is prepared as follows:
A, the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
Sn+2CH2=CHCOOCH3+2HCL→(CH3COOCCH2CH2)2SnCL2
By 115 kilograms of acrylic acid methyl ester .s (content is: 99.0%, technical grade), 2.8 kilograms of concentration be 31% concentrated hydrochloric acid and
0.9 kg catalyst FeCl3Add in chlorination enamel reaction still, start stirring, add 80 kilograms of glass putty (content while stirring
For: 99.99%, technical grade, mesh number is: 400 mesh), it being passed through dry hydrogen chloride gas 60kg simultaneously, this gas is passed through reactor
Bottom, in order to improve response speed, controlling reaction temperature is 80 DEG C, in 3 hours response time, (takes after glass putty reacts completely
Sample observing response situation), the solids lowered the temperature, filter white, its composition is: in dichloro dimethoxycarbonyl ethyl tin compound
Mesosome, then the aqueous solution of urea 24 kilograms with 1% washs the acrylic acid methyl ester. of excess residual, refilters, is dried pure
Dichloro dimethoxycarbonyl ethyl tin compound intermediate 189.1KG, yield is 96%；
B, the preparation of oleic acid mercaptoethanol ester:
HOCH2CH2SH+CH3(CH2) 7CH=CH (CH2)7COOH→
HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+H20
By 60 kilograms of 2 mercapto ethanols (content: 99%, technical grade), 191 kilograms of oleic acid (content: 99%, technical grade),
4.5 kilograms of content be 93% concentrated sulphuric acid add in reaction kettle of the esterification, heat while stirring, when temperature is heated to 70 DEG C, instead
It is 2.5 hours between Ying Shi, obtains semi-finished product, be then again heated to 85 DEG C ,-0.096MPa under condition of negative pressure, control this temperature
Keeping 2.5 hours, then lower the temperature, filter to obtain oleic acid mercaptoethanol ester 255KG, yield is 98%.
C, the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
(CH3COOCCH2CH2)2SnCL2+2HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+2NH3.H2O→
By 120 kg dichloro dimethoxycarbonyl ethyl tin compound intermediate, 210 kilograms of oleic acid mercaptoethanol esters, content
Being 80 kilograms of ammonia of 20%, 120 kg deionized water and 0.8 kilogram of ion exchange resin 732 type catalyst add in synthesis reactor, control
Reaction temperature processed 65 DEG C, reacts 1.5 hours, then blowing, layering, and organic facies carries out decompression distillation again, decompression distillation
Control condition is: temperature: 85-90 DEG C；Negative pressure :-0.098MPa；Response time: 3.5 hours, then lower the temperature, filter, obtain two
Oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compound 315KG, yield is 96.5%.
Embodiment 4
Prepare two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds of following molecular formula:
It is prepared as follows:
A, the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
Sn+2CH2=CHCOOCH3+2HCL→(CH3COOCCH2CH2)2SnCL2
By 96 kilograms of acrylic acid methyl ester .s (content is: 99.0%, technical grade), 1.9 kilograms of concentration be 31% concentrated hydrochloric acid and
0.45 kg catalyst AlCl3Add in chlorination enamel reaction still, start stirring, add 62 kilograms of glass putty (content while stirring
For: 99.99%, technical grade, mesh number is: 400 mesh), it being passed through dry hydrogen chloride gas 40kg simultaneously, this gas is passed through reactor
Bottom, in order to improve response speed, controlling reaction temperature is 60 DEG C, in 3 hours response time, (takes after glass putty reacts completely
Sample observing response situation), the solids lowered the temperature, filter white, its composition is: in dichloro dimethoxycarbonyl ethyl tin compound
Mesosome, then the aqueous solution of urea 20 kilograms with 1% washs the acrylic acid methyl ester. of excess residual, refilters, is dried pure
Dichloro dimethoxycarbonyl ethyl tin compound intermediate 135.2KG, yield is 95.8%；
B, the preparation of oleic acid mercaptoethanol ester:
HOCH2CH2SH+CH3(CH2) 7CH=CH (CH2)7COOH→
HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+H20
By 55 kilograms of 2 mercapto ethanols (content: 99%, technical grade), 195 kilograms of oleic acid (content: 99%, technical grade),
3.6 kilograms of content be 93% concentrated sulphuric acid add in reaction kettle of the esterification, heat while stirring, when temperature is heated to 65 DEG C, instead
It is 2.2 hours between Ying Shi, obtains semi-finished product, be then again heated to 85 DEG C ,-0.096MPa under condition of negative pressure, control this temperature
Keeping 2 hours, then lower the temperature, filter to obtain oleic acid mercaptoethanol ester 225KG, yield is 98%.
C, the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
(CH3COOCCH2CH2)2SnCL2+2HSCH2CH2COO(CH2) 7CH=CH (CH2)7CH3+2NH3.H2O→
By 105 kg dichloro dimethoxycarbonyl ethyl tin compound intermediate, 216 kilograms of oleic acid mercaptoethanol esters, content
Being 85 kilograms of ammonia of 17%, 105 kg deionized water and 0.55 kilogram of ion exchange resin 213 type catalyst add in synthesis reactor,
Control reaction temperature 65 DEG C, react 1.5 hours, then blowing, layering, organic facies is carried out decompression distillation again, decompression distillation
Control condition be: temperature: 85-90 DEG C；Negative pressure :-0.098MPa；Response time: 3.5 hours, then lower the temperature, filter, obtain
Two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compound 290KG, yield is 96.5%.
Claims (8)
1. an oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compound, it is characterised in that molecular formula is:
The preparation method of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds the most according to claim 1,
It is characterized in that comprising the steps:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. that will measure, concentrated hydrochloric acid and catalyst add in chlorination enamel reaction still, start stirring, while stirring
Adding glass putty, the mesh number of glass putty is 400 mesh, is passed through dry hydrogen chloride gas simultaneously, controls reaction temperature and is 50-85 DEG C, treats
The solids after glass putty reacts completely, lowered the temperature, filter white, its composition is in the middle of dichloro dimethoxycarbonyl ethyl tin compound
Body, then the acrylic acid methyl ester. of excess residual is removed in the aqueous solution of urea washing by 0.5-4 mass %, refilters, is dried pure
Clean dichloro dimethoxycarbonyl ethyl tin compound intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 2 mercapto ethanol, oleic acid, catalyst adds in reaction kettle of the esterification, heats while stirring, when temperature is heated to 55-70 DEG C
Time, react 1-4 hour, obtain semi-finished product；Then it is again heated to 80-90 DEG C, under condition of negative pressure, controls this temperature and keep 1-3
Within individual hour, obtain oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
By A, step B prepare dichloro dimethoxycarbonyl ethyl tin compound intermediate, oleic acid mercaptoethanol ester, ammonia, go from
Sub-water and catalyst add in synthesis reactor, control reaction temperature and are 60-70 DEG C, react 1-3 hour, then blowing, layering, will have
Machine carries out decompression distillation the most again, and what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.05-0.90MPa, reaction
Time: 3-4 hour, the final products then lower the temperature, filtered.
The preparation method of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds the most according to claim 2,
It is characterized in that comprising the steps:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. that will measure, concentrated hydrochloric acid and catalyst add in chlorination enamel reaction still, start stirring, while stirring
Adding glass putty, the mesh number of glass putty is: 400 mesh, is passed through dry hydrogen chloride gas simultaneously, controls reaction temperature and is 50-85 DEG C, treats
The solids after glass putty reacts completely, lowered the temperature, filter white, its composition is in the middle of dichloro dimethoxycarbonyl ethyl tin compound
Body, then the acrylic acid methyl ester. of excess residual is removed in the aqueous solution of urea washing by 0.5-2.5 mass %, refilters, is dried
Pure dichloro dimethoxycarbonyl ethyl tin compound intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 2 mercapto ethanol, oleic acid, catalyst adds in reaction kettle of the esterification, heats while stirring, when temperature is heated to 60-75 DEG C
Time, react 1.5-2.5 hour, obtain semi-finished product；Then it is again heated to 80-90 DEG C, under condition of negative pressure, controls this temperature and keep
Within 1.5-3 hour, obtain oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
By A, step B prepare dichloro dimethoxycarbonyl ethyl tin compound intermediate, oleic acid mercaptoethanol ester, ammonia, go from
Sub-water and catalyst add in synthesis reactor, control reaction temperature and are 60-65 DEG C, react 1.5 hours, then blowing, layering, will have
Machine carries out decompression distillation the most again, and what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.08-0.5MPa, during reaction
Between: 3-4 hour, the final products then lower the temperature, filtered.
4. according to the preparation side of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds described in claim 2,3
Method, it is characterised in that comprise the steps:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. of 60-120 kilogram, the concentrated hydrochloric acid of 1-3 kilogram and 0.1-1.0 kg catalyst are added chlorination enamel anti-
Answering in still, start stirring, add 50-80 kilogram of glass putty while stirring, the mesh number of glass putty is: 400 mesh, is passed through dry simultaneously
30-70 kilogram of hydrogen chloride gas, controls reaction temperature and is 50-85 DEG C, after glass putty reacts completely, lower the temperature, filter white
Solids, its composition is dichloro dimethoxycarbonyl ethyl tin compound intermediate, then water-soluble with the carbamide of 0.5-2.5 mass %
The acrylic acid methyl ester. of excess residual is removed in liquid 20kg washing, refilters, is dried to obtain pure dichloro dimethoxycarbonyl ethyl stannum
Compound intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 40-60 kilogram of 2 mercapto ethanol, 160-200 kilogram of oleic acid, 2-5 kg catalyst adds in reaction kettle of the esterification, while stir
Mix limit heating, when temperature is heated to 60-75 DEG C, reacts 1.5-2.5 hour, obtain semi-finished product；Then 80-90 it is again heated to
DEG C, under condition of negative pressure, control this temperature and keep 1.5-3 hour obtaining oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
The 80-120 kilogram of dichloro dimethoxycarbonyl ethyl tin compound intermediate that A, step B are prepared, 180-220 kilogram of oleic acid
Mercaptoethanol ester, deionized water 80-120kg, the ammonia of content 10-20% 60-100 kilogram and 0.5 kg catalyst add conjunction
Become in still, control reaction temperature and be 60-65 DEG C, react 1.5 hours, then blowing, layering, organic facies is carried out decompression again and steams
Evaporating, what decompression was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.08-0.1MPa, the response time: 3-4 hour, then
Cooling, the final products filtered.
5. according to the preparation side of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds described in claim 2,3
Method, it is characterised in that comprise the steps:
A. the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
The acrylic acid methyl ester. of 80-100 kilogram, the concentrated hydrochloric acid of 1.5-2.5 kilogram and 0.5 kg catalyst are added chlorination enamel anti-
Answering in still, start stirring, add 55-70 kilogram of glass putty while stirring, the mesh number of glass putty is: 400 mesh, is passed through dry 44 simultaneously
Kilogram hydrogen chloride gas, controls reaction temperature and is 50-85 DEG C, the solid after glass putty reacts completely, lowered the temperature, filter white
Thing, its composition is dichloro dimethoxycarbonyl ethyl tin compound intermediate, then with the aqueous solution of urea of 0.5-2.5 mass %
The acrylic acid methyl ester. of excess residual is removed in 21kg washing, refilters, is dried to obtain pure dichloro dimethoxycarbonyl ethyl stannum chemical combination
Thing intermediate；
B. the preparation of oleic acid mercaptoethanol ester
By 45-55 kilogram of 2 mercapto ethanol, 170-190 kilogram of oleic acid, 3-4 kg catalyst adds in reaction kettle of the esterification, while stir
Mix limit heating, when temperature is heated to 60-75 DEG C, reacts 1.5-2.5 hour, obtain semi-finished product；Then 80-90 it is again heated to
DEG C, under condition of negative pressure, control this temperature and keep 1.5-3 hour obtaining oleic acid mercaptoethanol ester；
C. the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
The 90-100 kilogram of dichloro dimethoxycarbonyl ethyl tin compound intermediate that A, step B are prepared, 190-210 kilogram of oleic acid
Mercaptoethanol ester, deionized water 100kg, the ammonia of content 10-20% 70-90 kilogram and 0.5 kg catalyst add synthesis reactor
In, control reaction temperature and be 60-65 DEG C, react 1.5 hours, then blowing, layering, organic facies is carried out decompression distillation again, subtracts
What pressure was distilled control condition is temperature: 80-95 DEG C, negative pressure: 0.08-0.1MPa, the response time: 3-4 hour, then cooling,
The final products filtered.
6. according to the preparation side of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds described in claim 2-5
Method, it is characterised in that a diameter of DN100 of described chlorination enamel reaction still, cylinder height: 4000mm, inside has hydrogen chloride gas
Conduit 3850mm, mixing speed is 450 revs/min, and has sampling observation panel, thermometer mouth and gauge port.
7. according to the preparation side of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds described in claim 2-5
Method, it is characterised in that described catalyst is AlCl3、FeCl3, ion exchange resin: 732 types or 213 types (commercially available prod: east, Bangbu is stood
Chemical Co., Ltd. produces).
8. the preparation method of an oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compound, it is characterised in that molecular formula
For:
It is prepared as follows:
A, the preparation of dichloro dimethoxycarbonyl ethyl tin compound intermediate
By 92 kilograms of acrylic acid methyl ester .s, 2 kilograms of concentration be 31% concentrated hydrochloric acid and 0.5 kilogram of AlCl3Add chlorination enamel reaction still
In, starting stirring, add 60 kilograms of glass puttys while stirring, be passed through dry hydrogen chloride gas 37kg simultaneously, this gas is passed through instead
Answering bottom portion, controlling reaction temperature is 60 DEG C, in 3 hours response time, after glass putty reacts completely, lowers the temperature, filters white
Solids, its composition is: dichloro dimethoxycarbonyl ethyl tin compound intermediate, and then the aqueous solution of urea 20 with 1% is public
The acrylic acid methyl ester. of jin washing excess residual, refilter, be dried in the middle of pure dichloro dimethoxycarbonyl ethyl tin compound
Body 132.1KG, yield is 95%；
B, the preparation of oleic acid mercaptoethanol ester:
By 50 kilograms of 2 mercapto ethanols, 181 kilograms of oleic acid, 3.5 kilograms of content be 93% concentrated sulphuric acid add in reaction kettle of the esterification,
Heating while stirring, when temperature is heated to 65 DEG C, the response time is 2.2 hours, obtains semi-finished product, is then again heated to 85
DEG C ,-0.096MPa under condition of negative pressure, control this temperature and keep 2 hours, then lower the temperature, filter to obtain oleic acid mercaptoethanol ester
215KG, yield is 98%；
C, the preparation of two oleic acid mercaptoethyl alcohol ester dimethoxycarbonyl ethyl tin compounds
By 100 kilograms of dichloro dimethoxycarbonyl ethyl tin compound intermediate, 206 kilograms of oleic acid mercaptoethanol esters, content is
80 kilograms of ammonia of 17%, 100 kilograms of deionized waters, 0.5 kilogram of ion exchange resin 213 type adds in synthesis reactor, controls reaction temperature
Spend 65 DEG C, react 1.5 hours, then blowing, layering, by organic facies again carry out decompression distillation, decompression distillation control condition
For: temperature: 85-90 DEG C, negative pressure :-0.098MPa；Response time: 3.5 hours, then lower the temperature, filter, obtain two oleic acid sulfydryls
Ethyl alcohol ester dimethoxycarbonyl ethyl tin compound 281KG, yield is 96.5%.
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| CN1088930A (en) * | 1993-10-12 | 1994-07-06 | 泰安市精细化工总厂 | Stable organotin compound and its production and application |
| CN1137048A (en) * | 1995-05-27 | 1996-12-04 | 深圳泛胜塑胶助剂有限公司 | PVC resin preparing process using mixture of methyl tin and thiolate as thermal stabilizer |
| CN1435416A (en) * | 2002-01-28 | 2003-08-13 | 朱雅文 | Dimercaptoacetate isooctyl ester dimethoxy-carbonylethyl-tin and preparing process thereof |
| CN102796282A (en) * | 2012-08-21 | 2012-11-28 | 衢州建华东旭助剂有限公司 | Aliphatic acid mercaptoethanol ester methyl tin heat stabilizer and preparation method thereof |
| CN104629208A (en) * | 2013-11-14 | 2015-05-20 | 湖北南星化工总厂 | Composite solid methyltin PVC (polyvinyl chloride) heat stabilizer and preparation method thereof |
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2016
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088930A (en) * | 1993-10-12 | 1994-07-06 | 泰安市精细化工总厂 | Stable organotin compound and its production and application |
| CN1137048A (en) * | 1995-05-27 | 1996-12-04 | 深圳泛胜塑胶助剂有限公司 | PVC resin preparing process using mixture of methyl tin and thiolate as thermal stabilizer |
| CN1435416A (en) * | 2002-01-28 | 2003-08-13 | 朱雅文 | Dimercaptoacetate isooctyl ester dimethoxy-carbonylethyl-tin and preparing process thereof |
| CN102796282A (en) * | 2012-08-21 | 2012-11-28 | 衢州建华东旭助剂有限公司 | Aliphatic acid mercaptoethanol ester methyl tin heat stabilizer and preparation method thereof |
| CN104629208A (en) * | 2013-11-14 | 2015-05-20 | 湖北南星化工总厂 | Composite solid methyltin PVC (polyvinyl chloride) heat stabilizer and preparation method thereof |
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