CN103333197A - Method for preparing silane coupling agent for water-based coating - Google Patents
Method for preparing silane coupling agent for water-based coating Download PDFInfo
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- CN103333197A CN103333197A CN2013102433099A CN201310243309A CN103333197A CN 103333197 A CN103333197 A CN 103333197A CN 2013102433099 A CN2013102433099 A CN 2013102433099A CN 201310243309 A CN201310243309 A CN 201310243309A CN 103333197 A CN103333197 A CN 103333197A
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Abstract
The invention discloses a method for preparing a silane coupling agent for a water-based coating. The method comprises the following steps of: adding allyl glycidyl ether and anhydrous ethanol into a reaction kettle, and then adding a compound catalyst; and heating the reaction kettle, dropwise adding triethoxysilane when the temperature reaches 58 to 60 DEG C, continuously heating to 60-80 DEG C, distilling under reduced pressure after reaction, thus obtaining the silane coupling agent product for the water-based coating. According to the method, ethanol is used as a solvent for controlling the reaction temperature to 60 and 80 DEG C, so that the generation quantity of silane coupling agent isomers in the reaction process is reduced, and the purity of the silane coupling agent product is over 98 percent; by selecting a new cheap catalyst for compounding, the consumption of chloroplatinic acid is reduced, and the production cost is reduced; and the compound catalyst has a good catalytic effect, and also reduces the initial temperature of the reaction to 58 to 60 DEG C.
Description
Technical field
The present invention relates to the preparation method of the silane coupling agent that a kind of water-borne coatings uses.Relate in particular to the preparation method of the silane coupling agent that a kind of Platinic chloride usage quantity water-borne coatings few, that temperature of reaction is low, product purity is high uses.
Background technology
The coating of China's production at present is based on oil paint basically, oil paint needs in a large number with an organic solvent, like this environment and HUMAN HEALTH there is bigger injury, also need the raw material that uses a large amount of petroleum resources or obtained by refining of petroleum in the production process of oil paint, also increased production cost virtually.Present environmental protection coating material is water-borne coatings, the thinner of water-borne coatings is water, it does not all have injury to environment and human body, in water-borne coatings, use organo silane coupling agent can improve the advection of filming, smooth property, non-stick property, water tolerance, chemical-resistant, high thermal resistance, anti-stain characteristic and printability resistance etc. significantly, existing water-borne coatings is to use simple Platinic chloride to make catalyzer with the preparation method of silane coupling agent, the consumption of Platinic chloride is big, because Platinic chloride is expensive, is necessary to study a kind of catalyzer and replaces Platinic chloride to reduce production costs.Temperature of reaction among the existing preparation method is also higher, generally is conducive to the generation of silane coupling agent isomer under 80 ~ 100 ℃ of these temperature, causes the amount of the silane coupling agent isomer in the products obtained therefrom bigger than normal, has had influence on the performance of water-borne coatings.
Summary of the invention
The present invention proposes the preparation method of the silane coupling agent that a kind of water-borne coatings uses, and this method is used new catalyst compounded, has reduced temperature of reaction, has reduced the usage quantity of Platinic chloride, has reduced production cost, has also improved product purity simultaneously.
In order to solve the prior art problem, the present invention is achieved by the following technical solutions.
The preparation method of the silane coupling agent that a kind of water-borne coatings is used, its step is as follows:
(1) Platinic chloride, triphenyl phosphorus or tetrahydrofuran (THF), Virahol are Platinic chloride by weight ratio: mix triphenyl phosphorus or tetrahydrofuran (THF): Virahol=1:0.5 ~ 10:90 ~ 100, obtains catalyst compounded after mixing;
(2) glycidyl allyl ether and dehydrated alcohol are joined in the reactor for glycidyl allyl ether: dehydrated alcohol=1:0.5 ~ 1 by weight ratio, add prepare in the step (1) catalyst compounded then in reactor, catalyst compounded add-on is 0.002 ~ 0.009 times of glycidyl allyl ether weight;
(3) reactor is carried out heat temperature raising, when temperature reaches 58 ~ 60 ℃, in reactor, drip triethoxyl silane, reaction is thermopositive reaction, size with quantity of reflux is controlled rate of addition, the add-on of triethoxyl silane is 1.2 ~ 2.0 times of glycidyl allyl ether weight, and reaction is carried out underpressure distillation after finishing, and namely obtains the silane coupling agent product that water-borne coatings is used.
Temperature of reaction control in the step (3) behind the adding triethoxyl silane is between 60 ~ 80 ℃, and the reaction times is 6 ~ 10h.
Temperature when the boiling point of liquid refers to that its vapour pressure equals ambient pressure, therefore the boiling point of liquid changes with the variation of ambient pressure, reduce intrasystem pressure by means of vacuum pump, just can reduce the boiling point of liquid, be the theoretical foundation of underpressure distillation, described underpressure distillation is the common method of separating the purification organic compound.In the distillation procedure process, because of the boiling point height of product, and at air distillation meeting polymerization reaction take place, therefore need to adopt the underpressure distillation mode to distill.
Under the condition of catalyst compounded existence, the present invention is undertaken by following reaction principle.
The main reaction equation is:
The side reaction equation is:
The present invention uses ethanol to control temperature of reaction as solvent, temperature control can well reduce the generation of silane coupling agent isomer in the reaction process between 60 ~ 80 ℃, the amount of silane coupling agent isomer in the gained silane coupling agent product is reduced, and the purity of silane coupling agent product reaches more than 98%; The present invention uses new catalyst compounded simultaneously, composite to reduce the usage quantity of Platinic chloride by selecting cheap catalyzer to carry out, and then reduced production cost, and catalyst compounded catalytic effect of the present invention is good, also the starting temperature of reaction is reduced to 58 ~ 60 ℃ simultaneously.
Embodiment
The present invention has disclosed the basic preparation method of the silane coupling agent that a kind of water-borne coatings uses, and its step is as follows:
(1) Platinic chloride, triphenyl phosphorus or tetrahydrofuran (THF), Virahol are Platinic chloride by weight ratio: mix triphenyl phosphorus or tetrahydrofuran (THF): Virahol=1:0.5 ~ 10:90 ~ 100, obtains catalyst compounded after mixing;
(2) glycidyl allyl ether and dehydrated alcohol are joined in the reactor for glycidyl allyl ether: dehydrated alcohol=1:0.5 ~ 1 by weight ratio, add prepare in the step (1) catalyst compounded then in reactor, catalyst compounded add-on is 0.002 ~ 0.009 times of glycidyl allyl ether weight;
(3) reactor is carried out heat temperature raising, when temperature reaches 58 ~ 60 ℃, in reactor, drip triethoxyl silane, reaction is thermopositive reaction, size with quantity of reflux is controlled rate of addition, the add-on of triethoxyl silane is 1.2 ~ 2.0 times of glycidyl allyl ether weight, and reaction is carried out underpressure distillation after finishing, and namely obtains the silane coupling agent product that water-borne coatings is used.
Temperature of reaction control in the step (3) behind the adding triethoxyl silane is between 60 ~ 80 ℃, and the reaction times is 6 ~ 10h.
Under the condition of catalyst compounded existence, the present invention is undertaken by following reaction principle.
The main reaction equation is:
The side reaction equation is:
For those skilled in the art's understanding, below with reference to specific embodiment preparation method of the present invention is described in further detail.
Embodiment 1
(1) Platinic chloride, triphenyl phosphorus, Virahol are Platinic chloride by weight ratio: triphenyl phosphorus: Virahol=1:0.5:90 mixes, and obtains catalyst compounded after mixing;
(2) glycidyl allyl ether and dehydrated alcohol are joined in the reactor for glycidyl allyl ether: dehydrated alcohol=1:0.5 by weight, add the catalyst compounded of above-mentioned preparation then in reactor, catalyst compounded addition is 0.002 times of glycidyl allyl ether weight;
(3) reactor is carried out heat temperature raising, when temperature reaches 58 ℃, beginning drips triethoxyl silane in reactor, reaction is thermopositive reaction, controls rate of addition with the size of quantity of reflux, the add-on of triethoxyl silane is 1.2 times of glycidyl allyl ether weight, reaction beginning heat release, the control rate of addition controls temperature of reaction at 60 ~ 65 ℃, carry out underpressure distillation after reacting 10h with this understanding, obtain the silane coupling agent product that water-borne coatings is used.
The silane coupling agent product purity that present embodiment gained water-borne coatings is used detects, and the purity that obtains the silane coupling agent that water-borne coatings uses is 98.9%.
Embodiment 2
(1) with Platinic chloride, tetrahydrofuran (THF), Virahol by weight ratio for Platinic chloride: tetrahydrofuran (THF): Virahol=1:5:95 mix obtain catalyst compounded;
(2) glycidyl allyl ether and dehydrated alcohol are joined in the reactor for glycidyl allyl ether: dehydrated alcohol=1:0.5 by weight, add the catalyst compounded of above-mentioned preparation then in reactor, catalyst compounded addition is 0.005 times of glycidyl allyl ether weight;
(3) reactor is carried out heat temperature raising, when temperature reaches 59 ℃, beginning drips triethoxyl silane in reactor, the add-on of triethoxyl silane is 1.6 times of glycidyl allyl ether weight, reaction beginning heat release, the control rate of addition controls temperature of reaction at 65 ~ 70 ℃, carry out underpressure distillation after reacting 7h with this understanding, obtain the silane coupling agent product that water-borne coatings is used.
The silane coupling agent product purity that present embodiment gained water-borne coatings is used detects, and the purity that obtains the silane coupling agent that water-borne coatings uses is 98.7%.
Embodiment 3
(1) with Platinic chloride, tetrahydrofuran (THF), Virahol by weight ratio for Platinic chloride: tetrahydrofuran (THF): Virahol=1:10:100 mix obtain catalyst compounded;
(2) with glycidyl allyl ether and dehydrated alcohol by weight joining in the reactor for glycidyl allyl ether: dehydrated alcohol=1:1, add in the reactor then and 0.009 times of glycidyl allyl ether identical weight catalyst compounded;
(3) reactor is carried out heat temperature raising, when temperature reaches 60 ℃, beginning drips triethoxyl silane in reactor, the add-on of triethoxyl silane is 2.0 times of glycidyl allyl ether weight, reaction beginning heat release, the control rate of addition controls temperature of reaction at 75 ~ 80 ℃, carry out underpressure distillation after reacting 6h with this understanding, obtain the silane coupling agent product that water-borne coatings is used.
The silane coupling agent product purity that present embodiment gained water-borne coatings is used detects, and the purity that obtains the silane coupling agent that water-borne coatings uses is 98.4%.
Embodiment 4
(1) with Platinic chloride, triphenyl phosphorus, Virahol by weight ratio for Platinic chloride: triphenyl phosphorus: Virahol=1:5:95 mix obtain catalyst compounded;
(2) glycidyl allyl ether and dehydrated alcohol are joined in the reactor for glycidyl allyl ether: dehydrated alcohol=1:0.5 by weight, add the catalyst compounded of above-mentioned preparation then in reactor, catalyst compounded addition is 0.005 times of glycidyl allyl ether weight;
(3) reactor is carried out heat temperature raising, when temperature reaches 60 ℃, beginning drips triethoxyl silane in reactor, the add-on of triethoxyl silane is 1.6 times of glycidyl allyl ether weight, reaction beginning heat release, the control rate of addition controls temperature of reaction at 75 ~ 80 ℃, carry out underpressure distillation after reacting 7h with this understanding, obtain the silane coupling agent product that water-borne coatings is used.
The silane coupling agent product purity that present embodiment gained water-borne coatings is used detects, and the purity that obtains the silane coupling agent that water-borne coatings uses is 98.5%.
The present invention uses ethanol to control temperature of reaction as solvent, temperature control can well reduce the generation of silane coupling agent isomer in the reaction process between 60 ~ 80 ℃, the growing amount of silane coupling agent isomer reduces in the gained silane coupling agent product, and the purity of silane coupling agent product reaches more than 98%; The present invention uses new catalyst compounded simultaneously, composite to reduce the usage quantity of Platinic chloride by selecting cheap catalyzer to carry out, and then reduced production cost, and catalyst compounded catalytic effect of the present invention is good, also the starting temperature of reaction is reduced to 58 ~ 60 ℃ simultaneously.
The content of mentioning in above-described embodiment is not to be limitation of the invention, and under the prerequisite that does not break away from inventive concept of the present invention, any apparent replacement is all within protection scope of the present invention.
Claims (2)
1. the preparation method of the silane coupling agent used of a water-borne coatings, its step is as follows:
(1) Platinic chloride, triphenyl phosphorus or tetrahydrofuran (THF), Virahol are Platinic chloride by weight ratio: mix triphenyl phosphorus or tetrahydrofuran (THF): Virahol=1:0.5 ~ 10:90 ~ 100, obtains catalyst compounded after mixing;
(2) glycidyl allyl ether and dehydrated alcohol are joined in the reactor for glycidyl allyl ether: dehydrated alcohol=1:0.5 ~ 1 by weight ratio, add the catalyst compounded of preparation in the step (1) then in the reactor, catalyst compounded add-on is 0.002 of glycidyl allyl ether weight ~ 0. 009 times;
(3) reactor is carried out heat temperature raising, when temperature reaches 58 ~ 60 ℃, in reactor, drip triethoxyl silane, reaction is thermopositive reaction, size with quantity of reflux is controlled rate of addition, the add-on of triethoxyl silane is 1.2 ~ 2.0 times of glycidyl allyl ether weight, and reaction is carried out underpressure distillation after finishing, and namely obtains the silane coupling agent product that water-borne coatings is used.
2. the preparation method of the silane coupling agent used of water-borne coatings according to claim 1 is characterized in that: add temperature of reaction control behind the triethoxyl silane in the step (3) between 60 ~ 80 ℃, the reaction times is 6 ~ 10h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112915047A (en) * | 2021-02-01 | 2021-06-08 | 浙江亦轩化妆品有限公司 | Anti-migration lip nourishing glaze |
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| CN101121723A (en) * | 2007-09-13 | 2008-02-13 | 湖北武大有机硅新材料股份有限公司 | Method for preparing gamma-(2,3-epoxypropoxy)propyltriethoxysilicane |
| CN101648967A (en) * | 2009-09-18 | 2010-02-17 | 湖北武大光子科技有限公司 | Preparation method of 3-(methacryloxypropyl) propyl-triethoxysilicane |
| CN102146091A (en) * | 2011-01-26 | 2011-08-10 | 湖北德邦化工新材料有限公司 | Bis-silane coupling agent and preparation method thereof |
| CN103146202A (en) * | 2013-03-18 | 2013-06-12 | 盐城菁华新材料科技有限公司 | Preparation method of liquid silicone rubber for packaging light-emitting diode |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101121723A (en) * | 2007-09-13 | 2008-02-13 | 湖北武大有机硅新材料股份有限公司 | Method for preparing gamma-(2,3-epoxypropoxy)propyltriethoxysilicane |
| CN101648967A (en) * | 2009-09-18 | 2010-02-17 | 湖北武大光子科技有限公司 | Preparation method of 3-(methacryloxypropyl) propyl-triethoxysilicane |
| CN102146091A (en) * | 2011-01-26 | 2011-08-10 | 湖北德邦化工新材料有限公司 | Bis-silane coupling agent and preparation method thereof |
| CN103146202A (en) * | 2013-03-18 | 2013-06-12 | 盐城菁华新材料科技有限公司 | Preparation method of liquid silicone rubber for packaging light-emitting diode |
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| 戴延凤等: "配位体在Ⅷ族金属催化硅氢加成反应中的作用", 《江西科学》, vol. 22, no. 4, 31 October 2004 (2004-10-31) * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112915047A (en) * | 2021-02-01 | 2021-06-08 | 浙江亦轩化妆品有限公司 | Anti-migration lip nourishing glaze |
| CN112915047B (en) * | 2021-02-01 | 2022-08-26 | 浙江亦轩化妆品有限公司 | Anti-migration lip nourishing glaze |
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Application publication date: 20131002 |