CN106008588A - Ultrafine dibutyltin oxide and preparation method thereof - Google Patents
Ultrafine dibutyltin oxide and preparation method thereof Download PDFInfo
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- CN106008588A CN106008588A CN201610372028.7A CN201610372028A CN106008588A CN 106008588 A CN106008588 A CN 106008588A CN 201610372028 A CN201610372028 A CN 201610372028A CN 106008588 A CN106008588 A CN 106008588A
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- dibutyltin oxide
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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 invention relates to an ultrafine dibutyltin oxide and a preparation method thereof, and belongs to the technical field of preparation of ultrafine powder catalysts. The preparation method concretely comprises the following steps: 1, heating dibutyltin dichloride to a certain temperature in order to liquefy dibutyltin dichloride , and introducing the liquefied dibutyltin dichloride to an atomizer; 2, starting the atomizer to atomize the liquid dibutyltin dichloride ; 3, spraying atomized dibutyltin dichloride flow into a reaction kettle equipped with an alkali liquid, fully mixing the flow with the alkali liquid, and carrying out a primary reaction; 4, separating the obtained liquid after the primary reaction ends, adding the alkali liquid, carrying out a secondary reaction, and carrying out a tertiary reaction; and 5, washing a material obtained in step 4 with water, centrifuging the washed material, carrying out vacuum drying, discharging the dried material, and weighing the discharged material to obtain the required ultrafine dibutyltin oxide product. Ultrafine dibutyltin oxide synthesized through the method is fine and uniform, has high purity, and can be used as an electrophoresis paint catalyst.
Description
Technical field
The invention belongs to the preparing technical field of superfine powder catalyst, be specifically related to a kind of ultra-fine Dibutyltin oxide and preparation method thereof.
Background technology
Dibutyltin oxide, English name Dibutyltin
Oxide, the white or faint yellow solid powder for one, mainly as the intermediate of production butyl tin series of heat stabilizer, and catalyst for esterification reaction, such as silicone rubber firming agent, polyester coating catalyst etc..
At present, the preparation method of Dibutyltin oxide uses the method being directly added dropwise to alkali liquor after being liquefied by dibutyl tin dichloride to be prepared, the preparation method as involved by patent CN101665510B.The product particle produced is big, and granule is uneven, is easily generated the shortcomings such as catalytic effect is the best, holiday is obvious, causes it cannot be applied in polyester coating, electrophoretic paint in coating industry is applied.
Summary of the invention
For solving the deficiency in above-mentioned existing product application technology, the present invention provides a kind of granule fine and smooth uniformly, ultra-fine Dibutyltin oxide that product purity is high and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is:
A kind of ultra-fine Dibutyltin oxide and preparation method thereof, comprises the following steps:
(1) dibutyl tin dichloride is heated to 40 DEG C-100 DEG C liquefy after import in nebulizer；(2) starting nebulizer makes liquid dibutyl tin dichloride be atomized；(3) spraying into the dibutyl tin dichloride air-flow after atomization equipped with in the reactor of alkali liquor, alkali liquor contains a small amount of surfactant, carries out first set reaction after being sufficiently mixed；(4) after completion of the reaction liquid separation is added alkali liquor and carry out second and third secondary response；(5) washing, be centrifuged, be vacuum dried, blowing is weighed and is obtained required ultra-fine Dibutyltin oxide product.
Further, the nebulizer used is supersonic atomizer or high-speed gas atomization device.
Further, water scouring water is deionized water.
Present invention have the advantage that
The present invention is by first carrying out being atomized the method carrying out reacting again with the alkali liquor containing surfactant by the dibutyl tin dichloride of liquid, make the Dibutyltin oxide granule generated during first set reaction fine and smooth uniformly, then by two, third-order reaction ensure dibutyl tin dichloride reaction thoroughly, water-washing process uses deionized water, ensure that the Dibutyltin oxide soluble ion concentration generated is low, finally give fine and smooth uniform product, fully meet electrophoretic paint coating and use requirement.
Detailed description of the invention
Below in conjunction with three experiment detailed description of the invention, the present invention will be further described; it is to be noted that implementation below is only the explanation type explanation being the present invention by way of example; but protection scope of the present invention is not limited to that, all those skilled in the art replace with the equivalence that the present invention is done by the spirit of the present invention and each fall within protection scope of the present invention.
Embodiment 1:
Weigh 24g sodium hydrate solid and put in 500ml four-hole boiling flask, dissolve with 150g water, add 4 surfactants standby, weigh 80g dibutyl tin dichloride to put into beaker is heated to 60 DEG C, slowly introduce in ultrasound atomizer and be atomized, unlatching flask stirs, and is introduced by atomization air flow glass tubing and carries out first set reaction under four-hole boiling flask alkali liquor liquid level at 1cm, and controlling reaction temperature is 60 DEG C.React complete sucking filtration except water, add 10g ammonia carry out two, third-order reaction.Deionized water washing, sucking filtration, be dried, finally give 63.5g Dibutyltin oxide product.Laboratory indexes is as follows: Sn:47.25%；Cl:0.0120%；Moisture ＜ 0.5%；350 mesh sieving rate ＞ 98%.
Embodiment 2:
Weigh 30g sodium hydrate solid and put in 1000ml beaker, dissolve with 200g water, add 6 surfactants, turn on agitator；Weighing 100g dibutyl tin dichloride and be heated to 70 DEG C, spray in beaker by air-current atomising device, control temperature is 70 DEG C and carries out first set reaction.React complete sucking filtration except water, add 10g ammonia carry out two, third-order reaction.Deionized water washing, sucking filtration, be dried, finally give 80.1g Dibutyltin oxide product.Laboratory indexes is as follows: Sn:47.36%；Cl:0.0090%；Moisture ＜ 0.5%；350 mesh sieving rate ＞ 95%.
Embodiment 3:
Weigh 10g sodium carbonate solid and put in 500ml four-hole boiling flask, dissolve with 200g water, adding 80g concentration is the ammonia of 20%, add 6 surfactants, turn on agitator, weighing 100g dibutyl tin dichloride and be heated to 65 DEG C, spray in beaker by air-current atomising device, control temperature is 45 DEG C and carries out first set reaction.React complete sucking filtration except water, add 10g ammonia carry out two, third-order reaction.Deionized water washing, sucking filtration, be dried, finally give 79.6g Dibutyltin oxide product.Laboratory indexes is as follows: Sn:47.23%；Cl:0.0076%；Moisture ＜ 0.5%；350 mesh sieving rate ＞ 98%.
Claims (3)
1. ultra-fine Dibutyltin oxide and preparation method thereof, it is characterised in that specifically include following steps: (1) dibutyl tin dichloride is heated to 40 DEG C-100 DEG C liquefy after import in nebulizer；(2) starting nebulizer makes liquid dibutyl tin dichloride be atomized；(3) spraying into the dibutyl tin dichloride air-flow after atomization equipped with in the reactor of alkali liquor, alkali liquor contains a small amount of surfactant, carries out first set reaction after being sufficiently mixed；(4) after completion of the reaction liquid separation is added alkali liquor and carry out second and third secondary response；(5) washing, be centrifuged, be vacuum dried, blowing is weighed and is obtained required ultra-fine Dibutyltin oxide product.
Ultra-fine Dibutyltin oxide of one the most according to claim 1 and preparation method thereof, it is characterised in that the nebulizer used is supersonic atomizer or high-speed gas atomization device.
Ultra-fine Dibutyltin oxide of one the most according to claim 1 and preparation method thereof, it is characterised in that water scouring water is deionized water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610372028.7A CN106008588B (en) | 2016-05-31 | 2016-05-31 | A kind of preparation method of Dibutyltin oxide |
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| CN201610372028.7A CN106008588B (en) | 2016-05-31 | 2016-05-31 | A kind of preparation method of Dibutyltin oxide |
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| CN106008588A true CN106008588A (en) | 2016-10-12 |
| CN106008588B CN106008588B (en) | 2019-01-18 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946928A (en) * | 2017-05-08 | 2017-07-14 | 南通艾德旺化工有限公司 | The preparation method of Dibutyltin oxide and its application in Sucralose synthesis |
| CN106977539A (en) * | 2017-05-22 | 2017-07-25 | 南通艾德旺化工有限公司 | A kind of preparation method of Mono-n-butyltin |
| CN107033182A (en) * | 2017-05-08 | 2017-08-11 | 南通艾德旺化工有限公司 | A kind of preparation method of Dibutyltin oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0276889A (en) * | 1988-06-03 | 1990-03-16 | Yoshitomi Pharmaceut Ind Ltd | Separation and preparation of alkyltin oxide |
| US4968823A (en) * | 1988-06-14 | 1990-11-06 | Yoshitomi Pharmaceutical Industries, Ltd. | Process for the fractional production of alkytin oxide |
| CN101665510A (en) * | 2009-08-03 | 2010-03-10 | 云南锡业锡化学品有限公司 | Preparation method of granular dibutyltin oxide |
| CN105540649A (en) * | 2016-01-27 | 2016-05-04 | 柳州豪祥特科技有限公司 | Preparation method of stannic oxide nanopowder |
-
2016
- 2016-05-31 CN CN201610372028.7A patent/CN106008588B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0276889A (en) * | 1988-06-03 | 1990-03-16 | Yoshitomi Pharmaceut Ind Ltd | Separation and preparation of alkyltin oxide |
| US4968823A (en) * | 1988-06-14 | 1990-11-06 | Yoshitomi Pharmaceutical Industries, Ltd. | Process for the fractional production of alkytin oxide |
| CN101665510A (en) * | 2009-08-03 | 2010-03-10 | 云南锡业锡化学品有限公司 | Preparation method of granular dibutyltin oxide |
| CN105540649A (en) * | 2016-01-27 | 2016-05-04 | 柳州豪祥特科技有限公司 | Preparation method of stannic oxide nanopowder |
Non-Patent Citations (2)
| Title |
|---|
| 袁福龙等: "用超声喷雾热分解法制备二氧化锡薄膜", 《黑龙江大学自然科学学报》 * |
| 陈玉祥: "超声波微波喷雾热解法制备氧化锡纳米粉体的研究", 《昆明理工大学专业学位硕士学位论文》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946928A (en) * | 2017-05-08 | 2017-07-14 | 南通艾德旺化工有限公司 | The preparation method of Dibutyltin oxide and its application in Sucralose synthesis |
| CN107033182A (en) * | 2017-05-08 | 2017-08-11 | 南通艾德旺化工有限公司 | A kind of preparation method of Dibutyltin oxide |
| CN106977539A (en) * | 2017-05-22 | 2017-07-25 | 南通艾德旺化工有限公司 | A kind of preparation method of Mono-n-butyltin |
| CN106977539B (en) * | 2017-05-22 | 2019-04-12 | 南通艾德旺化工有限公司 | A kind of preparation method of Mono-n-butyltin |
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| CN106008588B (en) | 2019-01-18 |
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Effective date of registration: 20190906 Address after: 661199 Metallurgical Materials Development Zone, Mengzi Economic and Technological Development Zone, Honghe Prefecture, Yunnan Province Patentee after: Yunnan Tin Industry Tin Chemical Materials Co., Ltd. Address before: 661099 Jinhu East Road, Honghe Hani and Yi Autonomous Prefecture, Yunnan, No. 121 East Road Patentee before: Yunnan Tin Chemical Company |
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