CN104497036A - Preparation technique of dibutyl tin diacetate - Google Patents
Preparation technique of dibutyl tin diacetate Download PDFInfo
- Publication number
- CN104497036A CN104497036A CN201410755664.9A CN201410755664A CN104497036A CN 104497036 A CN104497036 A CN 104497036A CN 201410755664 A CN201410755664 A CN 201410755664A CN 104497036 A CN104497036 A CN 104497036A
- Authority
- CN
- China
- Prior art keywords
- dibutyl tin
- tin acetate
- temperature
- heating
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000000034 method Methods 0.000 title abstract 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 34
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229960000583 acetic acid Drugs 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 10
- JJLKTTCRRLHVGL-UHFFFAOYSA-L [acetyloxy(dibutyl)stannyl] acetate Chemical compound CC([O-])=O.CC([O-])=O.CCCC[Sn+2]CCCC JJLKTTCRRLHVGL-UHFFFAOYSA-L 0.000 claims description 25
- 238000009413 insulation Methods 0.000 claims description 18
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000007664 blowing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- VIFFNYAVJACGFW-UHFFFAOYSA-N 2-butylhexanoic acid;tin Chemical compound [Sn].CCCCC(C(O)=O)CCCC VIFFNYAVJACGFW-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- LDZDQDDROJXUBO-UHFFFAOYSA-N acetic acid;dibutyltin Chemical compound CC(O)=O.CC(O)=O.CCCC[Sn]CCCC LDZDQDDROJXUBO-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Catalysts (AREA)
Abstract
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation technique of dibutyl tin diacetate. The technique comprises the following steps: (1) weighing excessive glacial acetic acid for reaction, and adding into reaction kettle; (2) starting a stirring device, and adding dibutyl tin oxide while stirring; (3) heating to 60-80 DEG C, and keeping the temperature to react for 1-2 hours until the dibutyl tin oxide is completely dissolved; (4) vacuumizing, heating to 105 DEG C, stopping heating, and keeping the temperature for 20-30 minutes; (5) continuing heating to 110 DEG C, keeping the temperature, and vacuumizing for 2-3.5 hours until no low-boiling-point substance is distilled off; and (6) discharging, and weighing to obtain the required dibutyl tin diacetate. The technique has the advantages of complete reaction, low production cost and good product quality.
Description
Technical field
The invention belongs to catalyst preparation technical field, be specifically related to a kind of dibutyl tin acetate preparation technology.
Background technology
Dibutyl tin acetate, English name Dibutyl tin diacetate, for light yellow or water white transparency is with the liquid of acetic acid smell, less than 10 DEG C in solid or semisolid, zero pour: 8 ~ 10 DEG C, density: 1.32 ± 0.005 (20 DEG C), boiling point: 140 ~ 144 DEG C/10mmHg.Main as room temperature silicon rubber curing catalysts, be especially applicable to the organosilicon goods of de-acetic acid type.Be characterized in that Catalysis Rate is fast, in order to reduce it acetic acid smell can with dibutyl tin laurate with the use of, expose and be easily hydrolyzed in atmosphere, bottleneck separates out solid, also can be used as polyurethane coating catalyzer.
Preparation method's many employings Glacial acetic acid of current acetic acid dibutyl tin is added in reactor with Dibutyltin oxide by certain mass ratio, and after reacting completely, the low-boiling-point substance such as removed under reduced pressure acetic acid, finally obtains dibutyl tin acetate.In traditional dibutyl tin acetate processing, product Theil indices is lower, cannot meet production requirement.And feeding quantity controls with great difficulty not cause more by product, reduces output, causes higher production cost, product quality reduces, easy crystallization etc.
Summary of the invention
For solving above-mentioned the deficiencies in the prior art, the present invention aims to provide that a kind of Theil indices is higher, and product reacts completely, and production cost is low, the preparation method of the dibutyl tin acetate of superior product quality.For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of dibutyl tin acetate preparation technology, specifically comprises the following steps:
(1) the required excessive Glacial acetic acid of reaction adds in reactor after weighing;
(2) open whipping appts, add Dibutyltin oxide while stirring;
(3) heat up, treat that temperature is increased between 60-80 DEG C, insulation reaction 1-2h, until Dibutyltin oxide all dissolves;
(4) vacuumize, heating, stop heating to temperature to 105 DEG C, insulation 20-30min;
(5) continuing to be heated to 110 DEG C, insulation, vacuumizing 2-3.5h to distillating without low-boiling-point substance;
(6) blowing is weighed and to be obtained required dibutyl tin acetate.
Concrete, the stanniferous amount of prepared dibutyl tin acetate is 27%-33.3%.
Concrete, described Glacial acetic acid is 4-6: 1 with the ratio of the amount of substance of Dibutyltin oxide.
Preferably, the stirring velocity in described step (2) is 150-250r/min.
The present invention adopts Glacial acetic acid and Dibutyltin oxide to carry out processing to react, and reaction process ensures that Glacial acetic acid is excessive, and reaction is carried out with stirring simultaneously, promotes to react completely, ensures product purity.Strict control temperature of reaction and reaction times, amount of by-products be reduced to minimum, the di-n-butylacetic acid tin purity that reaction generates is high, can to ensure in raw material that Dibutyltin oxide participates in reaction completely, makes Theil indices in product can up to 27%-33.3%.
Embodiment
Below in conjunction with embodiment, the present invention will be further described; it is to be noted that following embodiment is only the indicative explaination that the mode that exemplifies is done the present invention; but protection scope of the present invention is not limited in this, all those skilled in the art all fall into protection scope of the present invention with the replacement of spirit of the present invention to the equivalence that the present invention does.
Embodiment 1
A kind of dibutyl tin acetate preparation technology, specifically comprises the following steps:
(1) weighing 264g adds in reactor after Glacial acetic acid;
(2) open whipping appts, stirring velocity is 250r/min, adds 276g Dibutyltin oxide while stirring;
(3) heat up, treat that temperature is increased between 60-80 DEG C, insulation reaction 2h, all dissolves to Dibutyltin oxide;
(4) vacuumize, heating, stop heating to temperature to 105 DEG C, insulation 30min;
(5) continuing to be heated to 110 DEG C, insulation, vacuumizing 2h to distillating without low-boiling-point substance;
(6) blowing is weighed and to be obtained required dibutyl tin acetate.
Detecting Theil indices in prepared product is 27%.
Embodiment 2
A kind of dibutyl tin acetate preparation technology, comprises the following steps:
(1) weighing 320g Glacial acetic acid adds in reactor;
(2) open whipping appts, stirring velocity 200r/min, add 276g Dibutyltin oxide while stirring;
(3) heat up, treat that temperature is increased between 60-80 DEG C, insulation reaction 1.5h, until Dibutyltin oxide all dissolves;
(4) vacuumize, heating, stop heating to temperature to 105 DEG C, insulation 25min;
(5) continuing to be heated to 110 DEG C, insulation, vacuumizing 2.5h to distillating without low-boiling-point substance;
(6) blowing is weighed and to be obtained required dibutyl tin acetate.
The stanniferous amount of dibutyl tin acetate prepared by detection is 30%.
Embodiment 3
A kind of dibutyl tin acetate preparation technology, comprises the following steps:
(1) weighing 330g Glacial acetic acid adds in reactor;
(2) open whipping appts, control stirring velocity is 170r/min, adds 276g Dibutyltin oxide while stirring;
(3) heat up, treat that temperature is increased between 60-80 DEG C, insulation reaction 1.5h, until Dibutyltin oxide all dissolves;
(4) vacuumize, heating, stop heating to temperature to 105 DEG C, insulation 20min;
(5) continuing to be heated to 110 DEG C, insulation, vacuumizing 3.5h to distillating without low-boiling-point substance;
(6) blowing is weighed and to be obtained required dibutyl tin acetate.
Detecting Theil indices in products obtained therefrom is 33%.
Embodiment 4
A kind of dibutyl tin acetate preparation technology, comprises the following steps:
(1) weighing 396g Glacial acetic acid adds in reactor;
(2) open whipping appts, stirring velocity is 150r/min, adds 276g Dibutyltin oxide while stirring;
(3) heat up, treat that temperature is increased between 60-80 DEG C, insulation reaction 1.5h, until Dibutyltin oxide all dissolves;
(4) vacuumize, heating, stop heating to temperature to 105 DEG C, insulation 20min;
(5) continuing to be heated to 110 DEG C, insulation, vacuumizing 3.5h to distillating without low-boiling-point substance;
(6) blowing is weighed and to be obtained required dibutyl tin acetate.
In dibutyl tin acetate prepared by detection, Theil indices is 33.3%.
Claims (4)
1. a dibutyl tin acetate preparation technology, is characterized in that, specifically comprises the following steps: add in reactor after the required excessive Glacial acetic acid of (1) reaction weighs; (2) open whipping appts, add Dibutyltin oxide while stirring; (3) heat up, treat that temperature is increased between 60-80 DEG C, insulation reaction 1-2h, until Dibutyltin oxide all dissolves; (4) vacuumize, heating, stop heating to temperature to 105 DEG C, insulation 20-30min; (5) continuing to be heated to 110 DEG C, insulation, vacuumizing 2-3.5h to distillating without low-boiling-point substance; (6) blowing is weighed and to be obtained required dibutyl tin acetate.
2. a kind of dibutyl tin acetate preparation technology as claimed in claim 1, is characterized in that, the stanniferous amount of prepared dibutyl tin acetate is 27%-33.3%.
3. a kind of dibutyl tin acetate preparation technology as claimed in claim 1, is characterized in that, described Glacial acetic acid is 4-6: 1 with the ratio of the amount of substance of Dibutyltin oxide.
4. a kind of dibutyl tin acetate preparation technology as claimed in claim 1, is characterized in that, the stirring velocity in described step (2) is 150-250r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410755664.9A CN104497036A (en) | 2014-12-05 | 2014-12-05 | Preparation technique of dibutyl tin diacetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410755664.9A CN104497036A (en) | 2014-12-05 | 2014-12-05 | Preparation technique of dibutyl tin diacetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104497036A true CN104497036A (en) | 2015-04-08 |
Family
ID=52938506
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410755664.9A Pending CN104497036A (en) | 2014-12-05 | 2014-12-05 | Preparation technique of dibutyl tin diacetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104497036A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592564A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Preparation method of catalyst organotin acetate in sucralose production |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084861A (en) * | 1992-09-29 | 1994-04-06 | 北京化工三厂 | A kind of igelite thermo-stabilizer and preparation thereof |
| CN102516544A (en) * | 2011-11-23 | 2012-06-27 | 湖北新蓝天新材料股份有限公司 | Method for preparing dibutyltin dilaurate catalyst |
| CN102838631A (en) * | 2012-09-21 | 2012-12-26 | 沧州威达聚氨酯高科股份有限公司 | Synthesis method of dibutyltin dilaurate |
-
2014
- 2014-12-05 CN CN201410755664.9A patent/CN104497036A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084861A (en) * | 1992-09-29 | 1994-04-06 | 北京化工三厂 | A kind of igelite thermo-stabilizer and preparation thereof |
| CN102516544A (en) * | 2011-11-23 | 2012-06-27 | 湖北新蓝天新材料股份有限公司 | Method for preparing dibutyltin dilaurate catalyst |
| CN102838631A (en) * | 2012-09-21 | 2012-12-26 | 沧州威达聚氨酯高科股份有限公司 | Synthesis method of dibutyltin dilaurate |
Non-Patent Citations (1)
| Title |
|---|
| V.B. MOKAL等,: "Steric effects on the formation of isolable products in the reactions of dibutyltin oxides with carboxylic acids", 《JOURNAL OF ORGANOMETALLIC CHEMISTRY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592564A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Preparation method of catalyst organotin acetate in sucralose production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102295541B (en) | Preparation method of 3,3-dimethyl butyraldehyde | |
| CN101531775B (en) | Alkyl acyloxy silane mixture and preparation method thereof | |
| CN103275279B (en) | Disposable the feeding intake of normal temperature produces the method for polycarboxylate water-reducer | |
| CN102558559A (en) | Method of synthetizing small molecule hydroxyl silicone oil through using continuation method | |
| CN103849433A (en) | Automatic production technology of chlorinated paraffin | |
| CN102786689A (en) | Method for producing pharmaceutical dimeticone | |
| CN105237338A (en) | System and method for continuously synthesizing high-purity 3-chloro-1,2-propylene glycol | |
| CN104497036A (en) | Preparation technique of dibutyl tin diacetate | |
| CN103936711A (en) | Method for reducing moisture content of 1,3-propane sultone | |
| CN104447328B (en) | Method for preparing alkyl 4,4-difluoroacetylacetate | |
| CN102584522B (en) | Production method of 2,4-dichlorotoluene | |
| CN103193636A (en) | Method for synthetizing 2,3-butanediol ester | |
| CN111138268A (en) | Preparation method of 4,4' -biphenyldicarboxylic acid | |
| CN103484057A (en) | Preparation method of silicone resin for adhesion of solvent-free environment-friendly glass fiber | |
| CN202346934U (en) | Trimethoxy hydrogen silicon alcoholysis esterification pre-reaction device | |
| CN101700886B (en) | Method for preparing trichlorosilane from tetrachlorosilane | |
| CN104744250A (en) | Method for synthesizing diacetylglycine | |
| CN105801611A (en) | Methods for preparing phenyl silane and diphenyl silane | |
| CN103739843B (en) | Trichlorosilane silicon tetrachloride as by-product is utilized to produce the preparation technology of ethyl polysilicate | |
| CN101906111A (en) | Method for preparing methyl silicic acid and industrial hydrochloric acid by using hydrolysis of methyl trichlorosilane | |
| CN102161765B (en) | Organic silicon resin and preparation method thereof | |
| CN104447329A (en) | Preparation method of 2-chloroacetoacetic acid ethyl ester | |
| CN101544563A (en) | Preparation method of 2-methylcyclohexyl acetate | |
| CN111574388A (en) | Tranexamic acid and preparation method thereof | |
| CN104592283A (en) | Synthetic method of silane coupling agent Si-69 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150408 |
|
| WD01 | Invention patent application deemed withdrawn after publication |