CN104804034A - Preparation method of butyltin tris(2-ethylhexanoate) catalyst - Google Patents
Preparation method of butyltin tris(2-ethylhexanoate) catalyst Download PDFInfo
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- CN104804034A CN104804034A CN201510049486.2A CN201510049486A CN104804034A CN 104804034 A CN104804034 A CN 104804034A CN 201510049486 A CN201510049486 A CN 201510049486A CN 104804034 A CN104804034 A CN 104804034A
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Abstract
The invention discloses a preparation method of a butyltin tris(2-ethylhexanoate) catalyst. According to the preparation method, one step method is adopted, and the preparation method comprises following steps: butyltin trichloride and isocaprylic acid are delivered into a reactor for uniform stirring, an obtained mixture is heated to 40 to 60 DEG C, the temperature is maintained to be unchanged, an alkaline solution is slowly delivered into the reactor, and dropwise adding is controlled so as to obtain a mixed material with a pH value of 4.5 to 5.5; the temperature of the mixed material is controlled to be 60 to 90 DEG C, and the mixed material is allowed to stand for 30min so as to realize phase separation; drying under reduced pressure is carried out at a temperature lower than 90 DEG C, and filtration is carried out so as to obtain a light-yellow transparent liquid product. Purity of a butyltin tris(2-ethylhexanoate) product prepared via the preparation method can be higher than 98%. Technology optimization is realized without reducing catalyst activity; operation is simple; the preparation method is convenient to control; complete reaction of isocaprylic acid can be realized; raw material utilization ratio is relatively high; energy consumption is relatively low; material loss and energy waste are avoided; production cost is reduced; and side reactions are few.
Description
Technical field
The present invention relates to a kind of technology of preparing of monobutyl three isocaprylic acid tin catalyst, belong to organic synthesis field.
Background technology
Monobutyl three isocaprylic acid tin is a kind of catalyst for esterification reaction of efficient organic tin, there is resistant to hydrolysis and the high-quality characteristic such as add-on is few, catalytic activity is high, be mainly used in esterification and polycondensation that temperature of reaction is 210 ~ 240 DEG C, because catalyzer is in neutral, so to the corrosion-free effect of equipment, after completion of the reaction, without the need to separating thus not affecting end product quality.Be widely used in synthesizing produce powder coating, coil coating saturated resin and produce flexible PU foam and the aromatic polyol product etc. that hard bubbles.
Monobutyl-tin-trichloride reaction is normally first generated obtained Mono-n-butyltin product by the synthetic method of monobutyl three isocaprylic acid tin catalyst in the basic conditions, and then with Mono-n-butyltin product and isocaprylic acid carry out dehydration esterification reaction drying produces obtain, this method feature is that the water of meeting at substantial in Mono-n-butyltin production process carries out reacting and washing, centrifugal, drying process dust is large, risk is existed to operator ' s health, require higher to electrostatic protection, the rate of recovery is low.
Summary of the invention
The invention provides a kind of synthesize simple, be easy to control, the production method of monobutyl three isocaprylic acid tin catalyst that transformation efficiency is high.Eliminate the step that monobutyl-tin-trichloride is hydrolyzed in alkaline solution, produce without toxic dust, be beneficial to environment and health of human body, save water resources.
The technical solution used in the present invention is: a kind of preparation method of monobutyl three isocaprylic acid tin catalyst, comprises the following steps:
(1) measuring suitable quantity of water pours in four mouthfuls of reaction flasks, opens and stirs.Take in a certain amount of monobutyl-tin-trichloride reaction flask and stir, then take a certain amount of isocaprylic acid and add in reaction flask and stir.
(2) take the alkaline agent solution prepared and be placed in constant pressure funnel, control temperature slowly drips, and controls reaction end ph value, adds rear isothermal reaction.
(3) phase-splitting after leaving standstill, gas producing formation vacuumizes drying, filters.
Isocaprylic acid in step (1) and the mol ratio of monobutyl-tin-trichloride are that 3-3.3 is than 1.
In step (1), monobutyl-tin-trichloride and isocaprylic acid are uniformly mixed control temperature at 40 DEG C-60 DEG C
Alkaline reagents in step (2) is sodium carbonate, sodium hydroxide, ammoniacal liquor.
Control temperature in step (2) is 60 DEG C-90 DEG C.
Reaction end ph in step (2) is 4.5-5.5.
The isothermal reaction time in step (2) refers to 2h-4h.
In step (3), drying temperature is no more than 90 DEG C.
Raw material isocaprylic acid used and the purity requirement of monobutyl-tin-trichloride are not less than 98%.
Compared with prior art, tool of the present invention has the following advantages:
The inventive method employing monobutyl-tin-trichloride replaces Mono-n-butyltin to carry out reaction in the basic conditions with isocaprylic acid and prepares monobutyl three isocaprylic acid tin catalyst.
Production process of the present invention produces without toxic dust, eliminates the step that monobutyl-tin-trichloride in conventional production methods is hydrolyzed in basic solution, and waste water generation is few.
Present invention saves water resources protection environment and personnel safety, totally reduce energy consumption, shorten flow process.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
The preparation method of the monobutyl three isocaprylic acid tin catalyst that the embodiment of the present invention provides, comprises the following steps:
(1) measuring suitable quantity of water pours in four mouthfuls of reaction flasks, opens and stirs.Take in a certain amount of monobutyl-tin-trichloride reaction flask and stir, then take a certain amount of isocaprylic acid and add in reaction flask and stir.
(2) take the alkaline agent solution prepared and be placed in constant pressure funnel, control temperature slowly drips, and controlling reaction end ph value is 4.5-5.5, adds rear isothermal reaction 3h.
(3) leave standstill phase-splitting after 30 minutes, product heats up and vacuumizes drying, filters.
Be described in detail below by 9 specific embodiments.
Embodiment one:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.2g distilled water, add 108.3g monobutyl-tin-trichloride while stirring.Take 165.5g isocaprylic acid again to join constant temperature 40 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 50% aqueous sodium hydroxide solution, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 3, and after dripping, constant temperature 55 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 70 DEG C and carries out vacuum-drying, filters, obtains colourless transparent liquid finished product.
Yield reaches 95.4%, and product is limpid, and result of laboratory test is as follows: Theil indices 19.65% water-content 1.012% viscosity (20 DEG C) 73.01(mPas) Pt-Co 308
Embodiment two:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.5g monobutyl-tin-trichloride while stirring.Take 165.6g isocaprylic acid again to join constant temperature 50 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 50% aqueous sodium hydroxide solution, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 3, and after dripping, constant temperature 65 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 80 DEG C to carry out vacuumizing drying, filters, obtains light yellow transparent liquid finished product.
Reaction is comparatively complete, and yield reaches 94.3%.Result of laboratory test is as follows: Theil indices 19.75% water-content 0.893% viscosity (20 DEG C) 74.24(mPas) Pt-Co 343
Embodiment three:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.1g distilled water, add 108.5g monobutyl-tin-trichloride while stirring.Take 165.7g isocaprylic acid again to join constant temperature 60 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 50% aqueous sodium hydroxide solution, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 3, and after dripping, constant temperature 75 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 90 DEG C to carry out vacuumizing drying, filters, obtains light yellow clear liquid end product.
Result of laboratory test is as follows: Theil indices 19.88% water-content 0.341% viscosity (20 DEG C) 75.15(mPas) Pt-Co 357
Embodiment four:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.4g monobutyl-tin-trichloride while stirring.Take 165.5g isocaprylic acid again to join constant temperature 40 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 20% ammonia soln, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 4, and after dripping, constant temperature 65 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 70 DEG C to carry out vacuumizing drying, filters, obtains colourless transparent liquid finished product.
Tin recovery rate is high, reaches 98.1%, has a small amount of precipitation.Result of laboratory test is as follows: Theil indices 19.62% water-content 0.910% viscosity (20 DEG C) 72.33(mPas) Pt-Co 308
Embodiment five:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.5g monobutyl-tin-trichloride while stirring.Take 165.4g isocaprylic acid again to join constant temperature 50 DEG C in reaction flask and stir.
(2) in constant pressure funnel, adding content is 20% ammonia soln, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 5, and after dripping, constant temperature 65 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 60 DEG C to carry out vacuumizing drying, filters, obtains colourless transparent liquid finished product.
Embodiment six:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.4g monobutyl-tin-trichloride while stirring.Take 165.6g isocaprylic acid again to join constant temperature 60 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 20% ammonia soln, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 6, and after dripping, constant temperature 65 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 70 DEG C to carry out vacuumizing drying, filters, obtains colourless transparent liquid finished product.
Result of laboratory test is as follows: Theil indices 19.69% water-content 0.636% viscosity (20 DEG C) 79.35(mPas) Pt-Co 312
Embodiment seven:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.5g monobutyl-tin-trichloride while stirring.Take 165.5g isocaprylic acid again to join constant temperature 40 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 30% aqueous sodium carbonate, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 7, and after dripping, constant temperature 65 DEG C reacts 1h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 70 DEG C to carry out vacuumizing drying, filters, obtains colourless transparent liquid finished product.
React completely, yield reaches 93.7%, and product is limpid.Result of laboratory test is as follows: Theil indices 19.79% water-content 0.892% viscosity (20 DEG C) 83.16(mPas) Pt-Co 364
Embodiment eight:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.5g monobutyl-tin-trichloride while stirring.Take 165.6g isocaprylic acid again to join constant temperature 50 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 30% aqueous sodium carbonate, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 5, and after dripping, constant temperature 65 DEG C reacts 2h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 70 DEG C to carry out vacuumizing drying, filters, obtains colourless transparent liquid finished product.
Result of laboratory test is as follows: Theil indices 19.86% water-content 0.561% viscosity (20 DEG C) 74.68(mPas) Pt-Co 349
Embodiment nine:
(1) in the 1000mL flask being furnished with well heater, stirring, dropping funnel, once add 200.0g distilled water, add 108.5g monobutyl-tin-trichloride while stirring.Take 165.7g isocaprylic acid again to join constant temperature 60 degree in reaction flask and stir.
(2) in constant pressure funnel, adding content is 30% aqueous sodium carbonate, is slowly added dropwise to reaction flask, and controlling to drip terminal ph value is 5, and after dripping, constant temperature 65 DEG C reacts 3h again.
(3) leave standstill phase-splitting after 30 minutes, product is warming up to 70 DEG C to carry out vacuumizing drying, filters, obtains colourless transparent liquid finished product.
React completely, yield reaches 96.6%, and product is limpid, places nondiscoloration for a long time.
Claims (8)
1. a preparation method for monobutyl three isocaprylic acid tin catalyst, comprises the following steps: (1) takes a certain amount of distilled water and pours in four mouthfuls of reaction flasks and stir with monobutyl-tin-trichloride, and then adds reaction flask under taking isocaprylic acid agitation condition; (2) alkaline reagents is slowly added dropwise to reaction flask ph value to terminal, isothermal reaction; (3) phase-splitting after leaving standstill, gas producing formation decompression is empty dry, filters.
2. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: the isocaprylic acid in step (1) and the mol ratio of monobutyl-tin-trichloride are that 3-3.3 is than 1.
3. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: in step (1), monobutyl-tin-trichloride and isocaprylic acid are uniformly mixed control temperature at 40 DEG C-60 DEG C.
4. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: the alkaline reagents in step (2) is sodium carbonate, sodium hydroxide, ammoniacal liquor.
5. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: the control temperature in step (2) is 60 DEG C-90 DEG C.
6. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: the reaction end ph in step (2) is 4.5-5.5.
7. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: the isothermal reaction time in step (2) refers to 2h-4h.
8. the preparation method of a kind of monobutyl three isocaprylic acid tin as described in claim 1, is characterized in that: in step (3), drying temperature is no more than 90 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198929A (en) * | 2015-10-13 | 2015-12-30 | 云南锡业锡化学品有限公司 | Method for synthesizing butylhydroxyoxo-stannane |
| CN106279249A (en) * | 2016-07-20 | 2017-01-04 | 浙江海普顿新材料股份有限公司 | A kind of mixed anion methyl stannum and its preparation method and application |
| CN106883259A (en) * | 2017-02-17 | 2017-06-23 | 云南锡业股份有限公司化工材料分公司 | A kind of preparation method of oleic acid methyl tin |
| CN108350312A (en) * | 2015-09-25 | 2018-07-31 | 阿克佐诺贝尔国际涂料股份有限公司 | Thermoset composition, coating process and the method for producing japanning product |
| CN111499661A (en) * | 2020-04-13 | 2020-08-07 | 盘锦洪鼎化工有限公司 | Preparation method of tin oxide complex diisooctanoate |
| CN113816988A (en) * | 2021-10-25 | 2021-12-21 | 浙江禾本科技股份有限公司 | Synthetic method of triphenyl tin acetate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3167532A (en) * | 1960-06-06 | 1965-01-26 | M & T Chemicals Inc | Tin salts of p-vinylbenzoic acid, polymers thereof and process for preparing said salts |
| CN102099364A (en) * | 2008-05-15 | 2011-06-15 | 阿克马法国公司 | High purity monoalkyltin compounds and uses thereof |
-
2015
- 2015-02-01 CN CN201510049486.2A patent/CN104804034A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3167532A (en) * | 1960-06-06 | 1965-01-26 | M & T Chemicals Inc | Tin salts of p-vinylbenzoic acid, polymers thereof and process for preparing said salts |
| CN102099364A (en) * | 2008-05-15 | 2011-06-15 | 阿克马法国公司 | High purity monoalkyltin compounds and uses thereof |
Non-Patent Citations (1)
| Title |
|---|
| 吴亮: "三种有机锡化合物的合成", 《塑料助剂》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108350312A (en) * | 2015-09-25 | 2018-07-31 | 阿克佐诺贝尔国际涂料股份有限公司 | Thermoset composition, coating process and the method for producing japanning product |
| CN105198929A (en) * | 2015-10-13 | 2015-12-30 | 云南锡业锡化学品有限公司 | Method for synthesizing butylhydroxyoxo-stannane |
| CN106279249A (en) * | 2016-07-20 | 2017-01-04 | 浙江海普顿新材料股份有限公司 | A kind of mixed anion methyl stannum and its preparation method and application |
| CN106883259A (en) * | 2017-02-17 | 2017-06-23 | 云南锡业股份有限公司化工材料分公司 | A kind of preparation method of oleic acid methyl tin |
| CN111499661A (en) * | 2020-04-13 | 2020-08-07 | 盘锦洪鼎化工有限公司 | Preparation method of tin oxide complex diisooctanoate |
| CN113816988A (en) * | 2021-10-25 | 2021-12-21 | 浙江禾本科技股份有限公司 | Synthetic method of triphenyl tin acetate |
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