CN105329934A - Preparation method of hydrotalcite-like compound used for electrophoretic paint - Google Patents
Preparation method of hydrotalcite-like compound used for electrophoretic paint Download PDFInfo
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- CN105329934A CN105329934A CN201410404803.3A CN201410404803A CN105329934A CN 105329934 A CN105329934 A CN 105329934A CN 201410404803 A CN201410404803 A CN 201410404803A CN 105329934 A CN105329934 A CN 105329934A
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- houghite
- liquid
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- electrocoating paint
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Abstract
The invention discloses a preparation method of a hydrotalcite-like compound used for an electrophoretic paint. The method comprises the following steps: 1) dissolving nitrate of magnesium zinc aluminum in water, and labeling the product as a liquid A; 2) mixing sodium carbonate and sodium hydroxide, dissolving a mixture, and labeling the product as a liquid B; 3) dropping the liquid A and the liquid B simultaneously and synthesizing the hydrotalcite-like compound through a coprecipitation method, crystallizing the product for 8-10 hours in a high pressure reactor at temperature of 150-200 DEG C, or crystallizing the product for 60-90 hours in the high pressure reactor at temperature of 80-100 DEG C; 4) adding 1.5-3% of sodium stearate for modification; and 5) filtering a slurry, drying the slurry and crushing the material to obtain the white powder of the hydrotalcite-like compound. Compared with prior art, the preparation method of the hydrotalcite-like compound has the advantages of simple operation, energy consumption reduction, and easy realization of industrial production, and the obtained product has good anticorrosion, weather-resistance and toughening effects in the electrophoretic paint.
Description
Technical field
The present invention relates to the preparation field of houghite compound, exactly refer to a kind of preparation method of the houghite for electrocoating paint.
Background technology
Houghite compound (Hydrotalcite-likecompounds, HTlc) is the layered double hydroxide be made up of positively charged layers of metal hydroxides and interlayer charge balance anion.Available general formula is expressed as [M
2+(1-x) M
3+x (OH) 2] x+ [A
n-x/n] mH
2o, wherein M
2+be divalent metal, can Fe be had
2+, Co
2+, Cu
2+, Zn
2+, Mn
2+deng; M3+ is trivalent metal cation, can have Fe
3+, Cr
3+deng, by the efficient combination of these divalence and trivalent metal ion, two can be formed, the ternary even HTlcs of quaternary.A
n-for interlayer anion, can be inorganic anion as Cl
-, CO
3 2-deng; Also can be organic anion etc.; The negatively charged ion of A to be valence mumber be-n, X is M
3+with { M
3++ M
2+mol ratio.HTlc unit layer is parallel to each other and overlaps to form laminate structure, the structure of the every one deck in laminate structure and brucite Mg (OH)
2it is similar that (brucite is regular octahedron structure, and structure centre is Mg
2+, six summits are OH
-adjacent regular octahedron is interconnected to form lamella by hydroxyl common edge), to be interconnected by common edge by metal (hydrogen) oxygen octahedra to form, but chemical constitution is different from brucite, wherein part divalent-metal ion is replaced (being called isomorphous substitution) by trivalent metal ion, is called class brucite layer.
HTlc has the controllability of lamella chemical constitution, exchange and absorption property, acid-basicity, thermal decomposition performance, certain thermostability.When being heated to certain temperature, HTlc starts to decompose, and thermal decomposition process comprises middle water, lamella hydroxyl, the removing and the formation of cenotype of interlayer anion.HTlc thermolysis can form the metal oxide sosoloid with catalytic activity, and this is HTlc very important character.The HTlc thermostability of different metal composition is had nothing in common with each other.
At present, the synthetic method step of existing HTlc is numerous and diverse, operational difficulty, and power consumption is serious, and suitability for industrialized production is not easy to realize, and needs to improve.
Summary of the invention
For above-mentioned defect, the technical problem that the present invention solves is the preparation method providing a kind of houghite for electrocoating paint, simple to operate, reduces energy consumption, suitability for industrialized production is easy to realize, and the product obtained can well play the effects such as anticorrosion, weather-proof, toughness reinforcing in electrocoating paint.
In order to solve above technical problem, the preparation method of the houghite for electrocoating paint provided by the invention, comprises the steps:
(1) nitrate of magnesium zinc-aluminium is dissolved in water, be designated as A liquid;
(2) by sodium hydroxide and sodium carbonate mixed dissolution, B liquid is designated as;
(3) drip A liquid, B liquid by Co deposited synthesis houghite, crystallization 8-10h in the autoclave of 150-200 DEG C simultaneously;
(4) sodium stearate modification is added;
(5) by slurries filtration, drying, pulverizing, houghite white powder can be obtained.
Preferably, in step (1), the mol ratio of the nitrate of magnesium zinc-aluminium according to 1.9-2.1:0.2-0.4:1 is dissolved in water, is designated as A liquid, with the concentration of magnesium nitrate for 0.55-0.65mol/l.
Preferably, in step (2), by sodium hydroxide and sodium carbonate 3.5-4.5:1 mixed dissolution in molar ratio, be designated as B liquid, the concentration of sodium carbonate is 0.35-0.45mol/l.
Preferably, in step (4), adding massfraction is the modification of 1.5-3% sodium stearate.
Preferably, in step (5), by slurries filtration, drying, pulverizing, the houghite white powder of averageparticle at 1.5-3 micron can be obtained.In addition, the present invention, providing a kind of preparation method of the houghite for electrocoating paint, comprises the steps:
(1) nitrate of magnesium zinc-aluminium is dissolved in water, be designated as A liquid;
(2) by sodium hydroxide and sodium carbonate mixed dissolution, B liquid is designated as;
(3) drip A liquid, B liquid by Co deposited synthesis houghite, crystallization 60-90h in the autoclave of 80-100 DEG C simultaneously;
(4) sodium stearate modification is added;
(5) by slurries filtration, drying, pulverizing, houghite white powder can be obtained.
Preferably, in step (1), the mol ratio of the nitrate of magnesium zinc-aluminium according to 1.9-2.1:0.2-0.4:1 is dissolved in water, is designated as A liquid, with the concentration of magnesium nitrate for 0.55-0.65mol/l.
Preferably, in step (2), by sodium hydroxide and sodium carbonate 3.5-4.5:1 mixed dissolution in molar ratio, be designated as B liquid, the concentration of sodium carbonate is 0.35-0.45mol/l.
Preferably, in step (4), adding massfraction is the modification of 1.5-3% sodium stearate.
Preferably, in step (5), by slurries filtration, drying, pulverizing, the houghite white powder of averageparticle at 1.5-3 micron can be obtained.
Compared with prior art, the preparation method of the houghite for electrocoating paint of the present invention, has the following advantages:
1, processing step is simple, and cheaper starting materials is easy to get, and Granularity Distribution is even, reduces energy consumption, and suitability for industrialized production is easy to realize;
2, the product obtained can well play the effects such as anticorrosion, weather-proof, toughness reinforcing in electrocoating paint.
Accompanying drawing explanation
Fig. 1 is the schema for the preparation method of the houghite of electrocoating paint in the embodiment of the present invention.
Embodiment
In order to those skilled in the art can understand technical scheme provided by the present invention better, set forth below in conjunction with specific embodiment.
Refer to Fig. 1, this figure is the schema for the preparation method of the houghite of electrocoating paint in the embodiment of the present invention.
The preparation method of the houghite for electrocoating paint of the present invention, comprises the steps:
(1) mol ratio of the nitrate of magnesium zinc-aluminium according to 1.9-2.1:0.2-0.4:1 dissolved in water, be designated as A liquid, the concentration of magnesium nitrate is 0.55-0.65mol/l;
(2) by sodium hydroxide and sodium carbonate 3.5-4.5:1 mixed dissolution in molar ratio, be designated as B liquid, the concentration of sodium carbonate is 0.35-0.45mol/l;
(3) drip A liquid, B liquid by Co deposited synthesis houghite, crystallization 8-10h in the autoclave of 150-200 DEG C simultaneously;
(4) adding massfraction is the modification of 1.5-3% sodium stearate;
(5) by slurries filtration, drying, pulverizing, houghite white powder can be obtained.
In addition, the present invention reoffers a kind of preparation method of the houghite for electrocoating paint, comprises the steps:
(1) mol ratio of the nitrate of magnesium zinc-aluminium according to 1.9-2.1:0.2-0.4:1 dissolved in water, be designated as A liquid, the concentration of magnesium nitrate is 0.55-0.65mol/l;
(2) by sodium hydroxide and sodium carbonate 3.5-4.5:1 mixed dissolution in molar ratio, be designated as B liquid, the concentration of sodium carbonate is 0.35-0.45mol/l;
(3) drip A liquid, B liquid by Co deposited synthesis houghite, crystallization 60-90h in the autoclave of 80-100 DEG C simultaneously;
(4) adding massfraction is the modification of 1.5-3% sodium stearate;
(5) by slurries filtration, drying, pulverizing, houghite white powder can be obtained.
Embodiment 1
In the present embodiment, 31.6g magnesium nitrate Mg (NO is weighed
3)
26H
2o, 22.5g aluminum nitrate Al (NO3)
39H
2o and 5.0g zinc nitrate Zn (NO
3)
26H2O is dissolved in 133-150g pure water, and weighing 12.7g anhydrous sodium carbonate, 20g sodium hydroxide are fully dissolved in 133-150g pure water.Drip nitrate solution and alkali lye simultaneously.In the process dripped, pH value controls between 9.5, by maintenance temperature with stir constant ageing 1 hour after adding.To move in autoclave 180 DEG C of insulations 8 hours again, stir insulation simultaneously and terminate rear naturally cooling, take out the hydrotalcite slurry that ageing is good, add a certain amount of sodium stearate, react 2 hours at 80 DEG C of temperature, suction filtration, wash to specific conductivity and be less than drying, pulverize (sample obtained does initial analysis, comprises composition, XRD, granularity, BET).The houghite obtained adds in electrocoating paint by a certain percentage.
Embodiment 2
In the present embodiment, 83g magnesium nitrate Mg (NO is weighed
3)
26H
2o, 75g aluminum nitrate Al (NO3)
39H
2o and 14g zinc nitrate Zn (NO
3)
26H2O is dissolved in 450-600g pure water, and weighing 32g anhydrous sodium carbonate, 48g sodium hydroxide are fully dissolved in 450-600g pure water.Drip nitrate solution and alkali lye simultaneously.In the process dripped, pH value controls between 10, by maintenance temperature with stir constant ageing 1 hour after adding.To move in autoclave 150 DEG C of insulations 10 hours again, stir insulation simultaneously and terminate rear naturally cooling, take out the hydrotalcite slurry that ageing is good, add a certain amount of sodium stearate, react 2 hours at 80 DEG C of temperature, suction filtration, wash to specific conductivity and be less than drying, pulverize (sample obtained does initial analysis, comprises composition, XRD, granularity, BET).The houghite obtained adds in electrocoating paint by a certain percentage.
Embodiment 3
In the present embodiment, 83g magnesium nitrate Mg (NO is weighed
3)
26H
2o, 75g aluminum nitrate Al (NO3)
39H
2o and 14g zinc nitrate Zn (NO
3)
26H2O is dissolved in 450-600g pure water, and weighing 32g anhydrous sodium carbonate, 48g sodium hydroxide are fully dissolved in 450-600g pure water.Drip nitrate solution and alkali lye simultaneously.In the process dripped, pH value controls between 9.5, by maintenance temperature with stir constant ageing 1 hour after adding.To move in autoclave 80 DEG C of insulations 70 hours again, stir insulation simultaneously and terminate rear naturally cooling, take out the hydrotalcite slurry that ageing is good, add a certain amount of sodium stearate, react 2 hours at 80 DEG C of temperature, suction filtration, wash to specific conductivity and be less than drying, pulverize (sample obtained does initial analysis, comprises composition, XRD, granularity, BET).The houghite obtained adds in electrocoating paint by a certain percentage.
Embodiment 4
In the present embodiment, 31.6g magnesium nitrate Mg (NO is weighed
3)
26H
2o, 22.5g aluminum nitrate Al (NO3)
39H
2o and 5.0g zinc nitrate Zn (NO
3)
26H2O is dissolved in 133-150g pure water, and weighing 12.7g anhydrous sodium carbonate, 20g sodium hydroxide are fully dissolved in 133-150g pure water.Drip nitrate solution and alkali lye simultaneously.In the process dripped, pH value controls between 10, by maintenance temperature with stir constant ageing 1 hour after adding.To move in autoclave 100 DEG C of insulations 60 hours again, stir insulation simultaneously and terminate rear naturally cooling, take out the hydrotalcite slurry that ageing is good, add a certain amount of sodium stearate, react 2 hours at 80 DEG C of temperature, suction filtration, wash to specific conductivity and be less than drying, pulverize (sample obtained does initial analysis, comprises composition, XRD, granularity, BET).The houghite obtained adds in electrocoating paint by a certain percentage.
Compared with prior art, the preparation method of the houghite for electrocoating paint of the present invention, has the following advantages:
1, processing step is simple, and cheaper starting materials is easy to get, and Granularity Distribution is even, reduces energy consumption, and suitability for industrialized production is easy to realize;
2, the product obtained can well play the effects such as anticorrosion, weather-proof, toughness reinforcing in electrocoating paint.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. for a preparation method for the houghite of electrocoating paint, it is characterized in that, comprise the steps:
(1) nitrate of magnesium zinc-aluminium is dissolved in water, be designated as A liquid;
(2) by sodium hydroxide and sodium carbonate mixed dissolution, B liquid is designated as;
(3) drip A liquid, B liquid by Co deposited synthesis houghite, crystallization 8-10h in the autoclave of 150-200 DEG C simultaneously;
(4) sodium stearate modification is added;
(5) by slurries filtration, drying, pulverizing, houghite white powder can be obtained.
2. the preparation method of the houghite for electrocoating paint according to claim 1, it is characterized in that, in step (1), the mol ratio of the nitrate of magnesium zinc-aluminium according to 1.9-2.1:0.2-0.4:1 is dissolved in water, be designated as A liquid, with the concentration of magnesium nitrate for 0.55-0.65mol/l.
3. the preparation method of the houghite for electrocoating paint according to claim 1, it is characterized in that, in step (2), by sodium hydroxide and sodium carbonate 3.5-4.5:1 mixed dissolution in molar ratio, be designated as B liquid, the concentration of sodium carbonate is 0.35-0.45mol/l.
4. the preparation method of the houghite for electrocoating paint according to claim 1, is characterized in that, in step (4), adding massfraction is the modification of 1.5-3% sodium stearate.
5. the preparation method of the houghite for electrocoating paint according to claim 1, is characterized in that, in step (5), by slurries filtration, drying, pulverizing, can obtain the houghite white powder of averageparticle at 1.5-3 micron.
6. for a preparation method for the houghite of electrocoating paint, it is characterized in that, comprise the steps:
(1) nitrate of magnesium zinc-aluminium is dissolved in water, be designated as A liquid;
(2) by sodium hydroxide and sodium carbonate mixed dissolution, B liquid is designated as;
(3) drip A liquid, B liquid by Co deposited synthesis houghite, crystallization 60-90h in the autoclave of 80-100 DEG C simultaneously;
(4) sodium stearate modification is added;
(5) by slurries filtration, drying, pulverizing, houghite white powder can be obtained.
7. the preparation method of the houghite for electrocoating paint according to claim 6, it is characterized in that, in step (1), the mol ratio of the nitrate of magnesium zinc-aluminium according to 1.9-2.1:0.2-0.4:1 is dissolved in water, be designated as A liquid, with the concentration of magnesium nitrate for 0.55-0.65mol/l.
8. the preparation method of the houghite for electrocoating paint according to claim 6, it is characterized in that, in step (2), by sodium hydroxide and sodium carbonate 3.5-4.5:1 mixed dissolution in molar ratio, be designated as B liquid, the concentration of sodium carbonate is 0.35-0.45mol/l.
9. the preparation method of the houghite for electrocoating paint according to claim 6, is characterized in that, in step (4), adding massfraction is the modification of 1.5-3% sodium stearate.
10. the preparation method of the houghite for electrocoating paint according to claim 6, is characterized in that, in step (5), by slurries filtration, drying, pulverizing, can obtain the houghite white powder of averageparticle at 1.5-3 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410404803.3A CN105329934A (en) | 2014-08-15 | 2014-08-15 | Preparation method of hydrotalcite-like compound used for electrophoretic paint |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410404803.3A CN105329934A (en) | 2014-08-15 | 2014-08-15 | Preparation method of hydrotalcite-like compound used for electrophoretic paint |
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| CN105329934A true CN105329934A (en) | 2016-02-17 |
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| CN201410404803.3A Pending CN105329934A (en) | 2014-08-15 | 2014-08-15 | Preparation method of hydrotalcite-like compound used for electrophoretic paint |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441078A (en) * | 2018-04-19 | 2018-08-24 | 俞小峰 | A kind of anti-static and anti-corrosive paint and preparation method thereof |
| CN110255963A (en) * | 2019-06-14 | 2019-09-20 | 河海大学 | A kind of preparation method of modified houghite sulfate corrosion-resistance preservative for concrete |
| CN114229876A (en) * | 2021-12-24 | 2022-03-25 | 浙江丰虹新材料股份有限公司 | Process for producing hydrotalcite |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840568A (en) * | 2005-03-28 | 2006-10-04 | 同济大学 | Mg-Al hydrotalcite heat stabilizer and process for preparing same |
| CN1974399A (en) * | 2006-11-28 | 2007-06-06 | 山东大学 | Rod hydrotalcite-like compound and its prepn process |
| CN101942111A (en) * | 2009-07-06 | 2011-01-12 | 邵阳天堂助剂化工有限公司 | Preparation method and application of zinc-aluminum-magnesium hydrotalcite-based PVC complex heat stabilizer |
| CN102795657A (en) * | 2012-08-09 | 2012-11-28 | 福建师范大学 | Preparation method of white hydrotalcite-like compound |
-
2014
- 2014-08-15 CN CN201410404803.3A patent/CN105329934A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840568A (en) * | 2005-03-28 | 2006-10-04 | 同济大学 | Mg-Al hydrotalcite heat stabilizer and process for preparing same |
| CN1974399A (en) * | 2006-11-28 | 2007-06-06 | 山东大学 | Rod hydrotalcite-like compound and its prepn process |
| CN101942111A (en) * | 2009-07-06 | 2011-01-12 | 邵阳天堂助剂化工有限公司 | Preparation method and application of zinc-aluminum-magnesium hydrotalcite-based PVC complex heat stabilizer |
| CN102795657A (en) * | 2012-08-09 | 2012-11-28 | 福建师范大学 | Preparation method of white hydrotalcite-like compound |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441078A (en) * | 2018-04-19 | 2018-08-24 | 俞小峰 | A kind of anti-static and anti-corrosive paint and preparation method thereof |
| CN110255963A (en) * | 2019-06-14 | 2019-09-20 | 河海大学 | A kind of preparation method of modified houghite sulfate corrosion-resistance preservative for concrete |
| CN114229876A (en) * | 2021-12-24 | 2022-03-25 | 浙江丰虹新材料股份有限公司 | Process for producing hydrotalcite |
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Application publication date: 20160217 |