CN107056831A - A kind of high-purity Dibutyltin oxide preparation method - Google Patents
A kind of high-purity Dibutyltin oxide preparation method Download PDFInfo
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- CN107056831A CN107056831A CN201710034944.4A CN201710034944A CN107056831A CN 107056831 A CN107056831 A CN 107056831A CN 201710034944 A CN201710034944 A CN 201710034944A CN 107056831 A CN107056831 A CN 107056831A
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- dibutyltin oxide
- dibutyltin
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- 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 System
- C07F7/22—Tin compounds
- C07F7/2224—Compounds having one or more tin-oxygen linkages
Abstract
The present invention relates to a kind of preparation method of high-purity Dibutyltin oxide, the preparation technology uses dibutyltin chloride and alkali for raw material, synthetic reaction is carried out in organic solvent and aqueous solution heterogeneous system, centrifugation, drying is eventually passed and is prepared into Dibutyltin oxide finished product.Product purity prepared by the present invention is high, organic solvent and surfactant are used in preparation process as solvent and spe medium, the Dibutyltin oxide particle for generating quaternization is acted on during quaternization by SURFACTANT ADSORPTION to be transferred quickly in organic phase, so that product and the aqueous phase separation rich in chlorion, again by collecting the organic phase containing Dibutyltin oxide after multi_layer extraction, toluene is recovered by distillation, prepare high-purity Dibutyltin oxide, effectively chloride ion content≤50ppm in control product, reduces industrial water pollution.
Description
Technical field
The present invention relates to a kind of preparation method of Dibutyltin oxide, more particularly to a kind of high-purity low chlorine ion content
It is prepared by Dibutyltin oxide.
Background technology
Organotin is normally used for the production of the products such as polyurethane, particularly in polyurethane foam, coating, elastomer, glue
Extensive use in the industries such as glutinous agent, resin.Dibutyltin oxide can be applied to more as catalyst, heat stabilizer and intermediate
Field.Dibutyltin oxide is a kind of homogeneous surfactant of weakly acidic pH, reaction condition is gentle, yield is high, reaction speed is fast,
High effect nontoxic, to reaction vessel non-corrosiveness, have higher stereoselectivity and stability, hydrolytic resistance are good, be one
Plant the organotin surfactant of many industrial uses.Dibutyltin oxide can be used for polyvinyl chloride and organotin as heat stabilizer
In the production of the products such as plastics.Secondly, Dibutyltin oxide also can be used to prepare laurate two as the intermediate of excellent performance
The dibutyl system such as butyl tin, dibutyitin maleate, butyl maleate dibutyl tin class stabilizer.
The traditional production technology of Dibutyltin oxide is directly to be alkalized in aqueous, reacts the dibutyl oxygen of production
Change tin particles to be dispersed in aqueous phase, then produced by way of centrifugation, washing.
The domestic patent document on Dibutyltin oxide preparation is more, and for example patent CN 101665510B disclose one
The preparation method of granular dibutyltin oxide is planted, with dibutyltin chloride, sodium hydroxide solution, nertralizer and surface-active
Agent is that raw material prepares Dibutyltin oxide method, and product is graininess, and reaction is efficiently controllable, and chlorion contains in reaction product
Amount reaches 0.048%.Li Quan et al. discloses a kind of preparation modified technique of Dibutyltin oxide（The preparation of Dibutyltin oxide
Improve, Lee's congruence, Yunnan chemical, the 2nd phase of volume 29,2002）：Using dibutyltin chloride, sodium hydroxide solution, ether as original
Material prepares Dibutyltin oxide.Wu Liang discloses a kind of Synthesis for Dibutyl Tin Oxide（Synthesis for Dibutyl Tin Oxide
Process modification, Wu Liang, plastic additive, the 4th phase, 2007）：With sodium hydroxide, surfactant, solvent and Dibutyltin oxide
The content for preparing residual chlorine in Dibutyltin oxide, product for raw material is 0.025%.Patent CN105801619A discloses one kind with two
Dibutyl tin oxide, sodium hydroxide and surfactant（Toluene, normal heptane or ethanol）The system of Dibutyltin oxide is prepared for raw material
Standby technique.Patent CN106008588A is disclosed a kind of prepares ultra-fine Dibutyltin oxide with dibutyltin chloride and alkaline reaction
Chlorinity is 0.0120% in method, product.
Chloride ion content is 500ppm or so in the Dibutyltin oxide product of general technology production, so as to limit the production
Application of the product in higher-end businesses.Such as automobile electrophoretic paint coating application, the Dibutyltin oxide that electrophoresis process is used is a kind of excellent
Good catalyst, but chlorion is produced a very large impact to paint film and painting effect in electrophoretic paint coating process, thus require outer
Chloride ion content in portion's additive must be limited to relatively low scope.In order to break through the bottleneck of the application, many enterprises centrifugation,
The mode that the process of washing is washed by using massive laundering reduces in chloride ion content, optimal product index chloride ion content only
The near 80-100ppm of energy, and the water of process consumption and the wastewater flow rate of generation are the decades of times of output, seriously consume water resource,
Aggravate water pollution.
The content of the invention
High-purity Dibutyltin oxide is prepared the invention provides a kind of simple technique, is effectively reduced in process of production
Chloride ion content in the amount of bringing into of chlorion, reduction finished product, so as to solve application of the Dibutyltin oxide in high-end field.
In order to solve the above technical problems, the technical scheme is that：Use dibutyltin chloride and alkali for raw material, having
Carry out synthetic reaction in machine solvent and aqueous solution heterogeneous system, eventually pass centrifugation, drying be prepared into Dibutyltin oxide into
Product.Wherein, dibutyltin chloride：The mol ratio of alkali is 1:2-2.2.
Further, the high-purity Dibutyltin oxide synthesis step is：(1) dibutyltin chloride is dissolved in organic
In solvent, it is slowly added dropwise and is reacted into aqueous slkali；(2) the organic solvent layer containing product after quaternization is collected, added
To deionization water distillation, organic solvent is reclaimed；(3) by after part centrifugal of the residue containing water and product, drying, that is, this is prepared
The high-purity Dibutyltin oxide of invention.The minimum amount of organic solvent is the 80% of dibutyltin chloride mass fraction, no maximum
Limitation.The more reactions of solvent usage amount it is more uniform, but typically do not select too many solvent because during increase recycling design when
Between and energy consumption.
The aqueous slkali is one kind in sodium hydroxide, potassium hydroxide, ammoniacal liquor, alkali lye mass concentration 5-20%.
The organic solvent is aromatic series, cycloalkane or C6-8N-alkane solvent, such as the fragrant optional benzene of series solvent,
One kind in toluene, dimethylbenzene, cycloalkane can select hexamethylene, cyclooctane, and normal alkane can select normal heptane.Reactions steps
(2) depending on vapo(u)rizing temperature in is according to selected organic solvent.
In order to reach more preferable effect, surfactant can be used in synthesis, during the course of the reaction by the dibutyl of generation
The rapid absorption migration of granules of stannic oxide reduces the residence time in aqueous phase into organic phase, so that further chlorine in reduction finished product
Ion concentration.
Described surfactant is cationic, with following general structure：
Wherein, m values 5-20, n values 0-5.
Dosage of surfactant mass fraction used is the 0.5-1 ‰ of dibutyltin chloride quality in technique.Use with
The preparation method of upper body structure surface active agent, is characterized in that, dibutyltin chloride dissolves in organic solvent, is slowly added dropwise
Reacted into the aqueous slkali containing surfactant, eventually pass centrifugation, drying and be prepared into Dibutyltin oxide finished product.
The advantage of the invention is that：
(1) use organic solvent and surfactant as solvent and spe medium, pass through surface-active during quaternization
The Dibutyltin oxide particle that quaternization is generated is transferred quickly in organic phase by agent suction-operated, so that product is with being rich in
The aqueous phase separation of chlorion, then by the organic phase containing Dibutyltin oxide being collected after multi_layer extraction, be recovered by distillation first
Benzene, prepares high-purity Dibutyltin oxide, effectively chloride ion content≤50ppm in control product.
(2) substantial amounts of washing is not needed when Dibutyltin oxide finished product is centrifuged, and effectively save water resource reduces water
Pollution.Dosage of surfactant mass fraction used is only the 0.5-1 ‰ of dibutyltin chloride in technique, after distillation with
Dibutyltin oxide enters aqueous phase and is dissolved in water, and does not end up in finished product finally.
Embodiment
In order to deepen the understanding of the present invention, below the invention will be further described, the embodiment be only used for explain this
Invention, does not constitute the restriction to protection scope of the present invention.
Embodiment 1
607.4kg dibutyltin chlorides are dissolved in 500kg toluene, is instilled with 14kg/min speed and contains 1600kg mass
Concentration is in 10% sodium hydroxide and the solution of 0.4kg surfactants, wherein m takes in the molecular structural formula of surfactant
Value 10, n values 2.Temperature control continues stirring reaction at 50 DEG C, after dripping off 2 hours；
By the reaction solution stratification 1.5 hours after stirring reaction, isolate upper strata organic solvent layer and collect standby.In distillation
400kg deionized waters are added in device, 90 DEG C is heated to, the organic solvent containing Dibutyltin oxide is then added dropwise, are distilled to recover
Toluene solvant.Remaining aqueous phase prepares white Dibutyltin oxide powder 495.2kg by centrifuging, drying after distillation.
The yield of the present embodiment is 99.54%.
Embodiment 2
607.4kg dibutyltin chlorides are dissolved in 800kg toluene, is instilled with 14kg/min speed and contains 2240kg mass
Concentration is 10% potassium hydroxide, and temperature control continues stirring reaction at 45 DEG C, after dripping off 2.5 hours；
By the reaction solution stratification 2 hours after stirring reaction, isolate upper strata organic solvent layer and collect standby.In distiller
Middle addition 400kg deionized waters, are heated to 95 DEG C, and the organic solvent containing Dibutyltin oxide is then added dropwise, and are distilled to recover first
Benzene solvent.Remaining aqueous phase prepares white Dibutyltin oxide powder 493.4kg by centrifuging, drying after distillation.
The yield of the present embodiment is 99.18%.
Embodiment 3
607.4kg dibutyltin chlorides are dissolved in 650kg hexamethylenes, is instilled with 15kg/min speed and contains 1680kg matter
The sodium hydroxide that concentration is 10% is measured, temperature control continues stirring reaction at 50 DEG C, after dripping off 3 hours；
By the reaction solution stratification 2 hours after stirring reaction, isolate upper strata organic solvent layer and collect standby.In distiller
Middle addition 350kg deionized waters, are heated to 95 DEG C, and the organic solvent containing Dibutyltin oxide is then added dropwise, and are distilled to recover ring
Hexane solvent.Remaining aqueous phase prepares white Dibutyltin oxide powder 495.9kg by centrifuging, drying after distillation.
The yield of the present embodiment is 99.48%.
Embodiment 4
607.4kg dibutyltin chlorides are dissolved in 480kg hexamethylenes, is instilled with 15kg/min speed and contains 3440kg matter
Measure concentration for 5% sodium hydroxide and 0.45Kg surfactants solution in, wherein m in the molecular structural formula of surfactant
Value 10, n values 2.Temperature control continues stirring reaction at 50 DEG C, after dripping off 2 hours；
By the reaction solution stratification 1.5 hours after stirring reaction, isolate upper strata organic solvent layer and collect standby.In distillation
500kg deionized waters are added in device, 90 DEG C is heated to, the organic solvent containing Dibutyltin oxide is then added dropwise, are distilled to recover
Cyclohexane solvent.Remaining aqueous phase prepares white Dibutyltin oxide powder 495.1kg by centrifuging, drying after distillation.
The yield of the present embodiment is 99.52%.
Embodiment 5
607.4kg dibutyltin chlorides are dissolved in 750kg n-hexanes, is instilled with 15kg/min speed and contains 1026kg matter
Concentration is measured in 15% ammoniacal liquor and the solution of 0.6Kg surfactants, wherein m values in the molecular structural formula of surfactant
20, n values 5.Temperature control continues stirring reaction at 45 DEG C, after dripping off 3 hours；
By the reaction solution stratification 2 hours after stirring reaction, isolate upper strata organic solvent layer and collect standby.In distiller
Middle addition 500kg deionized waters, are heated to 95 DEG C, and the organic solvent containing Dibutyltin oxide is then added dropwise, and are distilled to recover just
Hexane solvent.Remaining aqueous phase prepares white Dibutyltin oxide powder 494.9kg by centrifuging, drying after distillation.
The yield of the present embodiment is 99.68%.
Embodiment 6
607.4kg dibutyltin chlorides are dissolved in 450kg n-hexanes, is instilled with 15kg/min speed and contains 1720kg matter
Measure concentration for 10% sodium hydroxide and 0.55Kg surfactants solution in, wherein m in the molecular structural formula of surfactant
Value 15, n values 5.Temperature control continues stirring reaction at 50 DEG C, after dripping off 2 hours；
By the reaction solution stratification 1.5 hours after stirring reaction, isolate upper strata organic solvent layer and collect standby.In distillation
500kg deionized waters are added in device, 90 DEG C is heated to, the organic solvent containing Dibutyltin oxide is then added dropwise, are distilled to recover
N-hexane solvent.Remaining aqueous phase prepares white Dibutyltin oxide powder 494.3kg by centrifuging, drying after distillation.
The yield of the present embodiment is 99.36%.
Product the key technical indexes is moisture, chloride ion content and Theil indices.Moisture measurement is according to national standard
Direct drying method is tested in GB5009.3-2010, and chloride ion content test is surveyed according in national standard GB/T15453-2008 moles of method
Examination.Theil indices test uses company standard, and method of testing is as follows：
The accurate certain mass that weighs is W1Dibutyltin oxide powder, be placed in drying (empty crucible into the crucible of constant weight
Weight W2), the 4-6mL concentrated sulfuric acids are added, 80 DEG C of heating 1h in convection oven is placed in, is subsequently placed in 400 DEG C of heating in Muffle furnace
0.5h, 800 DEG C of heating 2h, then take out and are cooled to room temperature weighing W3, Theil indices are calculated according to below equation：
Theil indices %=
Wherein, W1 weighs scope for 0.5-1g；0.7877 is the mass ratio of tin in Dibutyltin oxide.
Dibutyltin oxide product index prepared by embodiment is determined according to above method, it is as a result as follows：
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Moisture/% | 0.52% | 0.58% | 0.67% | 0.61% | 0.67% | 0.48% |
| Chlorion/ppm | 45 | 42 | 47 | 41 | 40 | 49 |
| Theil indices/% | 47.25% | 47.55% | 47.16% | 47.35% | 47.39% | 47.43% |
Data above shows that preparation method of the present invention can prepare the dibutyl oxidation of high-quality low chlorine ion content
Tin powder, cardinal principle is to use organic solvent and surfactant as solvent and spe medium, during quaternization
The Dibutyltin oxide particle for generating quaternization is acted on by SURFACTANT ADSORPTION to be transferred quickly in organic phase, so that
Make product and the aqueous phase separation rich in chlorion, then by collecting the organic phase containing Dibutyltin oxide after multi_layer extraction, lead to
Distillation recovery toluene is crossed, high-purity Dibutyltin oxide, effectively chloride ion content≤50ppm in control product is prepared.
The preparation technology is to use dibutyltin chloride and alkali for raw material, in organic solvent and aqueous solution heterogeneous system
Carry out synthetic reaction.
Use the effect of organic solvent：Dibutyltin chloride raw material is dissolved, it is general in the prior art to use ethanol or toluene
Class solvent.But use ethanol as solvent, just do not become heterogeneous system.It is advantageous in that using heterogeneous system, instead
The Dibutyltin oxide for answering process to generate（Particle, it is water insoluble）Can be in aqueous phase and the intermediate accumulation of organic boundary, it is to avoid
It is dispersed in water, reduces the contact area with chlorion.Documents CN105801619A method is identical with this method, is also
Using heterogeneous system, it is that alkali lye is added dropwise toward in toluene and dibutyltin chloride mixture to but differ in that documents,
The present invention is on the contrary, be that organic solvent and dibutyltin chloride mixture are added dropwise into alkali lye, it is to avoid material glues in course of reaction
It is thick, be conducive to reaction more abundant.
In order to reach more preferable effect, surfactant can be used in synthesis, the present invention is added in heterogeneous system
Surfactant, general Common surface activating agent is used（Toluene, normal heptane or ethanol）, and the surface that the present invention is used is lived
Property agent structural formula：, wherein, m values 5-20, n value 0-5.It has
Standby is the effect of absorption and phase transfer, and structure belongs to flocculant type.The action principle of surfactant of the present invention：It is first
The Dibutyltin oxide particle produced in course of reaction is adsorbed rapidly using charge adsorption effect, hydrophobicity is allowed to and further increases
By force；Dibutyltin oxide after adsorbed can be brought into and be dispersed in organic phase rapidly by the hydrophobic grouping of surfactant, thorough
Bottom is separated from the water, rather than only in aqueous phase and the intermediate accumulation of organic boundary.
The present invention does not need substantial amounts of washing when Dibutyltin oxide finished product is centrifuged, and effectively save water resource subtracts
Few water pollution.Dosage of surfactant mass fraction used is only the 0.5-1 ‰ of dibutyltin chloride in technique, after distillation
It is dissolved in water as Dibutyltin oxide enters aqueous phase, does not end up at finally in finished product, pass through during quaternization
The Dibutyltin oxide particle that SURFACTANT ADSORPTION effect generates quaternization is transferred quickly in organic phase, so that production
Product and the aqueous phase separation rich in chlorion, then by collecting the organic phase containing Dibutyltin oxide after multi_layer extraction, by steaming
Recovery toluene is evaporated, high-purity Dibutyltin oxide is prepared, effectively chloride ion content≤50ppm in control product reduces industry
Water pollution.
Claims (6)
1. a kind of high-purity Dibutyltin oxide preparation method, uses dibutyltin chloride and alkali for raw material, it is characterised in that：
Synthetic reaction is carried out in organic solvent and aqueous solution heterogeneous system, centrifugation, drying is eventually passed and is prepared into Dibutyltin oxide
Finished product, synthesis step is：(1) by dibutyltin chloride dissolving in organic solvent, it is slowly added dropwise and is reacted into aqueous slkali；
(2) the organic solvent layer containing product after quaternization is collected, add to deionization water distillation, reclaim organic solvent；(3) will
The remaining material centrifugation containing water and product, after drying, produce high-purity Dibutyltin oxide.
2. a kind of high-purity Dibutyltin oxide preparation method according to claim 1, it is characterised in that：In organic solvent
Add surfactant with aqueous solution heterogeneous system, by dibutyltin chloride dissolving in organic solvent, be slowly added dropwise to
Reacted in aqueous slkali containing surfactant, eventually pass centrifugation, drying and be prepared into Dibutyltin oxide finished product.
3. a kind of high-purity Dibutyltin oxide preparation method according to claim 2, it is characterised in that live on the surface
Property agent be cationic surface active agent, with following general structure：
Wherein, m values 5-20, n values 0-5.
4. a kind of high-purity Dibutyltin oxide preparation method according to claim 2, it is characterised in that used in technique
Dosage of surfactant mass fraction be dibutyltin chloride quality 0.5-1 ‰.
5. a kind of high-purity Dibutyltin oxide preparation method according to claim 1 or 2, it is characterised in that described
Aqueous slkali is one kind in sodium hydroxide, potassium hydroxide, ammoniacal liquor, and alkali lye mass concentration is 5-20%.
6. a kind of high-purity Dibutyltin oxide preparation method according to claim 1 or 2, it is characterised in that described to have
Machine solvent is aromatic series, cycloalkane or C6-8N-alkane solvent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710034944.4A CN107056831A (en) | 2017-01-18 | 2017-01-18 | A kind of high-purity Dibutyltin oxide preparation method |
| PCT/CN2017/075115 WO2018133174A1 (en) | 2017-01-18 | 2017-02-28 | Preparation method for high-purity dibutyltin oxide |
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| CN201710034944.4A CN107056831A (en) | 2017-01-18 | 2017-01-18 | A kind of high-purity Dibutyltin oxide preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018133174A1 (en) * | 2017-01-18 | 2018-07-26 | 江苏飞拓界面工程科技有限公司 | Preparation method for high-purity dibutyltin oxide |
| CN111253432A (en) * | 2020-03-23 | 2020-06-09 | 虹鼎国际化工(南通)有限公司 | Preparation method of low-conductivity dibutyltin oxide |
| CN113956283A (en) * | 2021-11-24 | 2022-01-21 | 云南锡业锡化工材料有限责任公司 | Method for synthesizing low-conductivity dibutyltin oxide by two-step method |
| CN115594710A (en) * | 2022-10-27 | 2023-01-13 | 上海沃凯生物技术有限公司（Cn） | Method for recovering dibutyltin oxide from inactivated tin-containing waste in sucralose industrial production |
| CN115594710B (en) * | 2022-10-27 | 2024-05-10 | 上海沃凯生物技术有限公司 | Method for recycling dibutyl tin oxide from deactivated tin-containing waste in industrial production of sucralose |
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| CN105601665A (en) * | 2015-12-30 | 2016-05-25 | 浙江新和成股份有限公司 | Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester |
| CN105801619A (en) * | 2016-04-13 | 2016-07-27 | 江苏鑫露化工新材料有限公司 | Preparation process of dibutyltin oxide |
| CN106083913A (en) * | 2016-06-14 | 2016-11-09 | 江苏飞拓界面工程科技有限公司 | A kind of organo-tin compound and synthetic method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101665510B (en) * | 2009-08-03 | 2012-11-14 | 云南锡业锡化学品有限公司 | Preparation method of granular dibutyltin oxide |
| CN107056831A (en) * | 2017-01-18 | 2017-08-18 | 江苏飞拓界面工程科技有限公司 | A kind of high-purity Dibutyltin oxide preparation method |
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2017
- 2017-01-18 CN CN201710034944.4A patent/CN107056831A/en active Pending
- 2017-02-28 WO PCT/CN2017/075115 patent/WO2018133174A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601665A (en) * | 2015-12-30 | 2016-05-25 | 浙江新和成股份有限公司 | Treatment method of dibutyltin oxide and application of treatment method to synthesis of cane sugar-6-ethyl ester |
| CN105801619A (en) * | 2016-04-13 | 2016-07-27 | 江苏鑫露化工新材料有限公司 | Preparation process of dibutyltin oxide |
| CN106083913A (en) * | 2016-06-14 | 2016-11-09 | 江苏飞拓界面工程科技有限公司 | A kind of organo-tin compound and synthetic method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018133174A1 (en) * | 2017-01-18 | 2018-07-26 | 江苏飞拓界面工程科技有限公司 | Preparation method for high-purity dibutyltin oxide |
| CN111253432A (en) * | 2020-03-23 | 2020-06-09 | 虹鼎国际化工(南通)有限公司 | Preparation method of low-conductivity dibutyltin oxide |
| CN113956283A (en) * | 2021-11-24 | 2022-01-21 | 云南锡业锡化工材料有限责任公司 | Method for synthesizing low-conductivity dibutyltin oxide by two-step method |
| CN113956283B (en) * | 2021-11-24 | 2023-12-19 | 云南锡业锡化工材料有限责任公司 | Method for synthesizing low-conductivity dibutyl tin oxide by two-step method |
| CN115594710A (en) * | 2022-10-27 | 2023-01-13 | 上海沃凯生物技术有限公司（Cn） | Method for recovering dibutyltin oxide from inactivated tin-containing waste in sucralose industrial production |
| CN115594710B (en) * | 2022-10-27 | 2024-05-10 | 上海沃凯生物技术有限公司 | Method for recycling dibutyl tin oxide from deactivated tin-containing waste in industrial production of sucralose |
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| Publication number | Publication date |
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| WO2018133174A1 (en) | 2018-07-26 |
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Application publication date: 20170818 |