CN102516544A - Method for preparing dibutyltin dilaurate catalyst - Google Patents
Method for preparing dibutyltin dilaurate catalyst Download PDFInfo
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- CN102516544A CN102516544A CN2011103745192A CN201110374519A CN102516544A CN 102516544 A CN102516544 A CN 102516544A CN 2011103745192 A CN2011103745192 A CN 2011103745192A CN 201110374519 A CN201110374519 A CN 201110374519A CN 102516544 A CN102516544 A CN 102516544A
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Abstract
The invention discloses a method for preparing a dibutyltin dilaurate catalyst. The method comprises the following steps of: adding lauric acid and dibutyl tin oxide, stirring, and heating, wherein when the temperature is raised to 50 DEG C, the reaction system has negative pressure; continuously heating to the temperature of between 80 and 88 DEG C, maintaining the temperature of the system, performing continuous reaction for 2 hours, stopping the negative pressure, adding acetic anhydride, and continuously reacting for 1 hour with stirring; and compounding the solution obtained by the reaction and auxiliary agents in a certain mass ratio, and thus obtaining a finished product. The method is optimized on the basis that the activity of the catalyst is not reduced, and is easy to operate and convenient to control; the lauric acid is basically completely reacted, so the utilization rate of the raw material is high, the energy consumption is relatively low, loss of the materials and waste of the energy are avoided, the production cost is reduced, and the side reaction is little; and the product is difficult to crystallize, and the freezing point of the product is obviously reduced.
Description
Technical field
The present invention relates to the Preparation of Catalyst field of room temperature vulcanized silicone rubber, particularly relate to a kind of preparation method of dibutyltin dilaurate catalyst.
Background technology
Dibutyl tin laurate (Dibutyltin dilaurate is called for short DBTDL) is the high boiling point multi-usage organotin catalysts of the special liquefaction processing of a kind of process, is colourless or light yellow oily liquid, and low temperature becomes the white crystals body.Dibutyl tin laurate is dissolved in most of usual vehicles and various industrial softening agent such as benzene, toluene, acetone, ETHYLE ACETATE, chloroform, tetracol phenixin, benzene, ethanol, sherwood oil; Water insoluble, be as the important component part of catalystsystem in the various chemical reactions.
Dibutyl tin laurate is not only at wood lacquer, PU (Polyurethane; Polyurethane(s) is called for short urethane) use as effective catalyst in the manufacturing of coating, metal ink, adhesive agent and sealing agent, can also be as catalyzer, acrylic elastomer and carboxylic rubber crosslinking reaction and the urethane foam synthetic catalyzer of Zylox; In addition; Also can be used in PVC (Polyvinylchloride, the SE) plastics, have efficient oilness and stability etc.; Consumption can obtain good catalytic effect between 0.01%～2%.
At present the preparation method of dibutyl tin laurate is: after LAURIC ACID 99 MIN and Dibutyltin oxide are fed intake according to the certain mass ratio; Begin to stir and heat up, when temperature arrived 60 ℃, reaction system began to be with negative pressure; Be warming up to 100-110 ℃ then, the entire reaction course time is 2.5h always.Owing to reasons such as above-mentioned reaction times, temperature of reaction, cause the LAURIC ACID 99 MIN reaction not exclusively, side reaction is many, causes problems such as higher, the easy crystallization of production cost.
Summary of the invention
The objective of the invention is provides a kind of preparation method of dibutyltin dilaurate catalyst in order to overcome the deficiency of above-mentioned background technology, on the basis that does not reduce catalyst activity, optimizes technology, simple to operate; Be convenient to control, and the LAURIC ACID 99 MIN primitive reaction is complete, raw material availability is higher; Energy consumption is lower, has avoided the loss of material and the waste of the energy, and production cost reduces; Side reaction is few, and product is difficult for crystallization, and zero pour obviously reduces.
The preparation method of dibutyltin dilaurate catalyst provided by the invention may further comprise the steps: A, stir after LAURIC ACID 99 MIN and Dibutyltin oxide fed intake and heat, when temperature was raised to 50 ℃, reaction system began to be with negative pressure; B, continuation heating are warming up to 80 ℃～88 ℃, and maintenance system temperature successive reaction 2h stops negative pressure then, adds acetic anhydride, continues stirring reaction 1h again; C, solution that reaction is obtained than compound auxiliary, finally obtain finished product according to certain mass.
In technique scheme, the mol ratio of LAURIC ACID 99 MIN described in the steps A and Dibutyltin oxide is 1.7～2: 1, is preferably 1.82～1.9: 1.
In technique scheme, compound auxiliary described in the step C is at least a in acetic acid, DOP, phenylate, dodecylbenzene, the Oleum Cocois.
In technique scheme, when the composite auxiliary agent of solution described in the step C comprised acetic acid, the mass percent of acetic acid and solution was 3%～3.5%.
In technique scheme, when the composite auxiliary agent of solution described in the step C comprised DOP, the mass percent of DOP and solution was 4%～8%.
In technique scheme, when the composite auxiliary agent of solution described in the step C comprised phenylate, the mass percent of phenylate and solution was 3%～9%.
In technique scheme, when the composite auxiliary agent of solution described in the step C comprised dodecylbenzene, the mass percent of dodecylbenzene and solution was 1%～2%.
In technique scheme, when the composite auxiliary agent of solution described in the step C comprised Oleum Cocois, the mass percent of Oleum Cocois and solution was 8.5%～9.1%.
Compared with prior art, advantage of the present invention is following:
(1) in the reaction process of the present invention, the LAURIC ACID 99 MIN primitive reaction is complete, and raw material availability is higher, and energy consumption is lower, has avoided the loss of material and the waste of the energy, and production cost reduces.
(2) temperature of reaction of the present invention is gentle, and side reaction is few.
(3) the present invention adds the dewatering agent acetic anhydride in reaction process, helps fully removing the moisture that dereaction generates, and product is difficult for crystallization.
(4) after the present invention reacted the product compound auxiliary of generation, it is liquid that product can keep under 2 ℃～4 ℃ environment for a long time, and the zero pour of product obviously reduces.
(5) the present invention optimizes technology on the basis that does not reduce catalyst activity, and is simple to operate, is convenient to control.
Embodiment
Below in conjunction with specific embodiment the present invention is made further detailed description.
The preparation method of the dibutyltin dilaurate catalyst that the embodiment of the invention provides may further comprise the steps:
A, be to feed intake (preferred molar ratio be 1.82～1.9: 1), stir also heating, when temperature be raised to 50 ℃, reaction system begin be with negative pressure at 1.7～2: 1 in molar ratio with LAURIC ACID 99 MIN and Dibutyltin oxide;
B, continuation heating are warming up to 80 ℃～88 ℃, and maintenance system temperature successive reaction 2h stops negative pressure then, adds acetic anhydride, continues stirring reaction 1h again;
C, solution that reaction is obtained than compound auxiliary, finally obtain finished product according to certain mass.Compound auxiliary is at least a in acetic acid, DOP (DOP), phenylate, dodecylbenzene, the Oleum Cocois, and when the composite auxiliary agent of solution comprised acetic acid, the mass percent of acetic acid and solution was 3%～3.5%; When the composite auxiliary agent of solution comprised DOP, the mass percent of DOP and solution was 4%～8%; When the composite auxiliary agent of solution comprised phenylate, the mass percent of phenylate and solution was 3%～9%; When the composite auxiliary agent of solution comprised dodecylbenzene, the mass percent of dodecylbenzene and solution was 1%～2%; When the composite auxiliary agent of solution comprised Oleum Cocois, the mass percent of Oleum Cocois and solution was 8.5%～9.1%.
Main chemical reactions formula in the embodiment of the invention is:
Be elaborated through 8 specific embodiments below.
Embodiment 1:
A, take by weighing LAURIC ACID 99 MIN 480g and Dibutyltin oxide 300g (mol ratio is 1.99: 1), place the 1000mL there-necked flask, begin then to stir and heat temperature raising.When temperature was raised to 50 ℃, system began to be with negative pressure;
B, continuation heating are warming up to 80 ℃, constantly take the moisture that reaction generates away through negative pressure, and maintenance system temperature successive reaction 2h stops negative pressure then, in there-necked flask, add a certain amount of acetic anhydride, continue stirring reaction 1h again;
After C, the cooling, get the solution that the 50g reaction obtains, add compound auxiliary: 1.8g acetic acid, 2.8gDOP and 5.4g Oleum Cocois (mass percent of acetic acid, DOP and Oleum Cocois and solution is respectively 3.0%, 4.7% and 9.0%) finally obtain finished product.Be that this finished product standing storage is difficult for crystallization under 2 ℃ the condition in temperature.
Embodiment 2:
In the present embodiment; Except that following situation is different from embodiment 1; All the other are with embodiment 1: take by weighing LAURIC ACID 99 MIN 460g and Dibutyltin oxide 300g (mol ratio is 1.91: 1) in the steps A; Heat temperature raising to 85 ℃ among the step B is got the 100g resultant of reaction among the step C, the compound auxiliary of adding is 9.0gDOP and 3.5g phenylate (mass percent of DOP and phenylate and solution is respectively 8.0% and 3.1%).
Embodiment 3:
In the present embodiment; Except that following situation is different from embodiment 2; All the other are with embodiment 2: take by weighing LAURIC ACID 99 MIN 450g and Dibutyltin oxide 300g (mol ratio is 1.86: 1) in the steps A, the compound auxiliary that adds among the step C is 5.0g phenylate and 2.1g dodecylbenzene (mass percent of phenylate and dodecylbenzene and solution is respectively 4.7% and 2.0%).
Embodiment 4:
In the present embodiment; Except that following situation is different from embodiment 2; All the other are with embodiment 2: take by weighing LAURIC ACID 99 MIN 440g and Dibutyltin oxide 300g (mol ratio is 1.82: 1) in the steps A; Heat temperature raising to 88 ℃ among the step B, the compound auxiliary that adds among the step C is 10.0g phenylate and 1.5g dodecylbenzene (mass percent of phenylate and dodecylbenzene and solution is respectively 9.0% and 1.3%).
Embodiment 5:
In the present embodiment; Except that following situation is different from embodiment 2; All the other are with embodiment 2: take by weighing LAURIC ACID 99 MIN 420g and Dibutyltin oxide 300g (mol ratio is 1.74: 1) in the steps A, the compound auxiliary that adds among the step C is 3.9g acetic acid and 9.0g phenylate (mass percent of acetic acid and phenylate and solution is respectively 3.5% and 8.0%).
Embodiment 6:
In the present embodiment, except that the compound auxiliary that adds is that 3.5g acetic acid and 1.2g dodecylbenzene (mass percent of acetic acid and dodecylbenzene and solution is respectively 3.3% and 1.1%) are different from the embodiment 3, all the other are with embodiment 3.
Embodiment 7:
In the present embodiment, except that the compound auxiliary that adds is that 4.6gDOP and 9.8g Oleum Cocois (mass percent of DOP and Oleum Cocois and solution is respectively 4.0% and 8.6%) are different from the embodiment 3, all the other are with embodiment 3.
Embodiment 8:
In the present embodiment, except that the compound auxiliary that adds is that 10.0g Oleum Cocois (mass percent of Oleum Cocois and solution is 9.1%) is different from the embodiment 3, all the other are with embodiment 3.
The finished product that the foregoing description 2～8 obtains is under 2 ℃～4 ℃ the condition, to place three days in temperature, solidification phenomenon all do not occur, is the normal liquid shape, and wherein the finished product that obtains of embodiment 7 is the most limpid, but the dark relatively point of color.
The activity of facing the dibutyltin dilaurate catalyst of embodiment of the invention preparation down detects.
Use dibutyl tin laurate catalysis tetraethoxy and hydroxy-end capped YSR 3286 (107 glue; About molecular weight 80,000) speed of response; Through measuring the surface skining time (surface drying time) of polymkeric substance, the different of surperficial completely solidified time (tack-free time) and integrally curing time confirm that catalytic activity just.
Get two prepared dibutyltin dilaurate catalyst products of prior art (buy two kinds) and do test sample, be numbered 1 and 2 from market; Do detection by embodiment 2,3,6,7,8 gained samples respectively, sample number into spectrum 3,4,5,6,7.
Get each 25g of black wash and tetraethoxy and join linking agent mutually; The catalyzer of white oil 27g and 3g numbering 1-9 is made into each catalyst solution of 10%, in 100g base glue, adds the catalyzer 2ml that joins linking agent 5g and 10% mutually again and stirs back detection its surface drying time, tack-free time and the completely solidified time.Experimental result sees table:
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Surface drying time (min) | 47 | 150 | 45 | 50 | 50 | 45 | 50 |
| Tack-free time (min) | 140 | 250 | 140 | 140 | 145 | 130 | 140 |
| The completely solidified time (h) | 5 | 20 | 6 | 5 | 5 | 4 | 4 |
[0052]Result by above form can find out that the dibutyltin dilaurate catalyst of embodiment of the invention preparation has moderate surface drying time, tack-free time and completely solidified time, better catalytic activity.
Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.The content of not doing in this specification sheets to describe in detail belongs to this area professional and technical personnel's known prior art.
Claims (9)
1. the preparation method of a dibutyltin dilaurate catalyst is characterized in that may further comprise the steps:
A, stir after LAURIC ACID 99 MIN and Dibutyltin oxide fed intake and heat, when temperature was raised to 50 ℃, reaction system began to be with negative pressure;
B, continuation heating are warming up to 80 ℃～88 ℃, and maintenance system temperature successive reaction 2h stops negative pressure then, adds acetic anhydride, continues stirring reaction 1h again;
C, solution that reaction is obtained than compound auxiliary, finally obtain finished product according to certain mass.
2. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 1, it is characterized in that: the mol ratio of LAURIC ACID 99 MIN described in the steps A and Dibutyltin oxide is 1.7～2: 1.
3. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 2, it is characterized in that: the mol ratio of said LAURIC ACID 99 MIN and Dibutyltin oxide is 1.82～1.9: 1.
4. like the preparation method of each described dibutyltin dilaurate catalyst in the claim 1 to 3, it is characterized in that: compound auxiliary described in the step C is at least a in acetic acid, DOP, phenylate, dodecylbenzene, the Oleum Cocois.
5. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 4, it is characterized in that: when the composite auxiliary agent of solution described in the step C comprised acetic acid, the mass percent of acetic acid and solution was 3%～3.5%.
6. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 4, it is characterized in that: when the composite auxiliary agent of solution described in the step C comprised DOP, the mass percent of DOP and solution was 4%～8%.
7. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 4, it is characterized in that: when the composite auxiliary agent of solution described in the step C comprised phenylate, the mass percent of phenylate and solution was 3%～9%.
8. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 4, it is characterized in that: when the composite auxiliary agent of solution described in the step C comprised dodecylbenzene, the mass percent of dodecylbenzene and solution was 1%～2%.
9. the preparation method of dibutyltin dilaurate catalyst as claimed in claim 4, it is characterized in that: when the composite auxiliary agent of solution described in the step C comprised Oleum Cocois, the mass percent of Oleum Cocois and solution was 8.5%～9.1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011103745192A CN102516544A (en) | 2011-11-23 | 2011-11-23 | Method for preparing dibutyltin dilaurate catalyst |
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| CN2011103745192A CN102516544A (en) | 2011-11-23 | 2011-11-23 | Method for preparing dibutyltin dilaurate catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104497036A (en) * | 2014-12-05 | 2015-04-08 | 长沙罗斯科技有限公司 | Preparation technique of dibutyl tin diacetate |
| CN107033184A (en) * | 2017-05-23 | 2017-08-11 | 南通艾德旺化工有限公司 | The preparation method and its product of a kind of dibutyl tin laurate |
| CN107163075A (en) * | 2017-07-24 | 2017-09-15 | 西北有色金属研究院 | A kind of synthetic method of dibutyl tin laurate |
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| US4559319A (en) * | 1984-03-26 | 1985-12-17 | Toshiba Silicone Co., Ltd. | Curing agent composition for silicone elastomers |
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| US4559319A (en) * | 1984-03-26 | 1985-12-17 | Toshiba Silicone Co., Ltd. | Curing agent composition for silicone elastomers |
Non-Patent Citations (3)
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| 《昭通师专学报》 19901231 罗家刚 直接烃基化法制备月桂酸二丁基锡 1-3 , 第9期 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102838631B (en) * | 2012-09-21 | 2015-04-29 | 沧州威达聚氨酯高科股份有限公司 | Synthesis method of dibutyltin dilaurate |
| CN104497036A (en) * | 2014-12-05 | 2015-04-08 | 长沙罗斯科技有限公司 | Preparation technique of dibutyl tin diacetate |
| CN107033184A (en) * | 2017-05-23 | 2017-08-11 | 南通艾德旺化工有限公司 | The preparation method and its product of a kind of dibutyl tin laurate |
| CN107033184B (en) * | 2017-05-23 | 2019-03-22 | 南通艾德旺化工有限公司 | A kind of preparation method and its product of dibutyl tin dilaurate |
| CN107163075A (en) * | 2017-07-24 | 2017-09-15 | 西北有色金属研究院 | A kind of synthetic method of dibutyl tin laurate |
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Application publication date: 20120627 |