CN110372021A - A kind of preparation method and application of electronic circuit board or electrician's fire retardant aluminium hydroxide - Google Patents
A kind of preparation method and application of electronic circuit board or electrician's fire retardant aluminium hydroxide Download PDFInfo
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- CN110372021A CN110372021A CN201910510604.3A CN201910510604A CN110372021A CN 110372021 A CN110372021 A CN 110372021A CN 201910510604 A CN201910510604 A CN 201910510604A CN 110372021 A CN110372021 A CN 110372021A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses the preparation method of a kind of electronic circuit board or electrician's fire retardant aluminium hydroxide, this method uses inorganic acid to react the aluminium hydroxide crystal seed that preparation activity is high, performance is stable with sodium aluminate solution first；Then the high-activity crystal seed prepared in advance is added portionwise into sodium aluminate solution at 65-75 DEG C, under stirring after insulation reaction 8-12h, filters pressing, washing obtain aluminum hydroxide filter cake；A certain proportion of modifying agent is added after filter cake mashing to be modified, modified product is dried to obtain final aluminum hydroxide product through drier.This preparation method simple process, it is easy to industrialized production.Aluminum hydroxide product granularity prepared by the present invention is controllable simultaneously, and temperature tolerance is high, and conductivity is low, and oil absorbency is low, can meet the application of electronic circuit board or electrician trade.
Description
Technical field
The present invention relates to a kind of electronic circuit board or electrician's preparation methods of fire retardant aluminium hydroxide, relate in particular to
A kind of process synthesizing aluminium hydroxide fire retardant, belongs to technical field of inorganic material synthesis.
Background technique
Aluminium hydroxide is mainly used for thermosetting plastics, thermoplastic, synthetic rubber, painting as a kind of inorganic fire retardants
The industries such as material, building materials and electrician.Electronic circuit board aluminium hydroxide, main purpose be it is fire-retardant for assisting, reduce cost.Now
The aluminium hydroxide of electronic circuit board mainly leans on import, such as SUMITOMO CHEMICAL, Showa electrician and the refined treasured in the U.S..Domestic
Aluminium hydroxide causes product quality poor, scientific and technological content is lower, is only applicable to building traffic skill due to lacking ultra-fine chemical industry kind
Art field of less demanding, the application in the high-tech areas such as the electronics industry more demanding to flame retardant performance, aviation is then
It is less.Therefore it is controllable to develop a kind of product granularity, temperature tolerance is high, and conductivity is low, and oil absorbency is low, can meet electronic circuit board or electricity
The aluminium hydroxide synthesis technology of the application of industrial and commercial bank's industry has biggish realistic meaning.
106745126 A of patent CN discloses a kind of with the method for phosphoric acid seed production ultrafine aluminium hydroxide.This method
Crystal seed is prepared with phosphoric acid, kind point-score prepares ultrafine aluminium hydroxide flame retardant products, and crystal seed preparation method is single in the technique, crystal seed
Additive amount is big, and addition manner is single, and the product of production is relatively single, therefore production cost is relatively high, using field by one
Definite limitation.
Patent CN101182020 B discloses a kind of preparation method of electrical-special aluminum hydroxide.This method is by aluminic acid
Sodium solution divides aluminium hydroxide coarse raw materials made from two methods by kind point, carbon respectively, mixes according to a certain percentage after crushed
Uniformly obtained electrical-special aluminum hydroxide, the technique is although simple and easy to do, but product is only used for the electrician trade of low side, nothing
Method is applied to higher-end businesses.
The present invention is primarily directed to the above problem, and using simple synthesis technology, preparing best in quality can be used for electronics
The fire retardant aluminium hydroxide of wiring board or electrician trade.
Summary of the invention
A kind of preparation method the object of the present invention is to provide electronic circuit board or electrician with fire retardant aluminium hydroxide, the party
Method simple process, production overall cost is low, easy to industrialized production.Aluminum hydroxide product granularity made from this method can simultaneously
Control, temperature tolerance is high, and conductivity is low, and oil absorbency is low, can meet the application of electronic circuit board or electrician trade.
The preparation method of a kind of electronic circuit board of the present invention or electrician's fire retardant aluminium hydroxide, including following step
It is rapid:
(1) aluminium hydroxide crystal seed that preparation activity is high, performance is stable is reacted with sodium aluminate solution using inorganic acid；
(2) crystal seed of above-mentioned preparation is added portionwise into sodium aluminate solution at 65-75 DEG C, is kept the temperature under stirring anti-
After answering 8-12h, filters pressing, washing obtain aluminum hydroxide filter cake；
(3) it a certain proportion of modifying agent is added is modified after filter cake mashing, modified product is dry through drier
To final aluminum hydroxide product.
Wherein: inorganic acid described in step (1) is one of nitric acid, sulfuric acid, glacial acetic acid.
Inorganic acid concentration (wt%) described in step (1) is 20-95%.
The content (AO) of sodium aluminate solution aluminum oxide employed in step (1) is 200-350g/L.
Reaction temperature involved in step (1) is 35-55 DEG C, and the pH of reaction end is 8-10, reaction time 0.5-
2h, product cut size are 0.6-1 μm.
Preferred above-mentioned inorganic acid is nitric acid, and concentration (wt%) is 40-65%, and sodium aluminate solution AO content is 240-
260g/L, reaction temperature are 40-50 DEG C, and reaction end pH is 8-9, reaction time 1h.
The content (AO) of sodium aluminate solution aluminum oxide employed in step (2) is 120-130g/L.
Crystal seed divides 1-4 addition in step (2), the time is added at the beginning of reaction between reaction 4h, seed is always than control
For 1-5%.
It is preferred that it is 1 time or 3 times that number, which is added, in crystal seed, seed is always 1.5-3.5% than control.
Modifying agent employed in step (3) is one or more of phosphoric acid, polyacrylic acid, ammonium dihydrogen phosphate.
The additive amount of modifying agent employed in step (3) is 2-7%.
Preferred above-mentioned modifying agent is ammonium dihydrogen phosphate, and modifying agent additive amount is 3-5%.
Aluminum hydroxide product granularity prepared by the present invention is controllable, product cut size (D50) between 1.5-5 μm, crystal seed can be passed through
Additional amount controls product granularity, 5% weightless temperature of product between 275-280 DEG C, oil absorbency in 15-30g/100g linseed oil,
Conductivity is in 10-30us/cm.
Aluminium hydroxide fire retardant prepared by the present invention can meet the requirement of electronic circuit board or electrician trade.
In conclusion beneficial effects of the present invention:
(1) preparation method simple process of the present invention, production overall cost is low, easy to industrialized production.
(2) aluminum hydroxide product size tunable prepared by the present invention, temperature tolerance is high, and conductivity is low, and oil absorbency is low, can meet
The requirement of electronic circuit board or electrician trade can be used for making high-end product.
Detailed description of the invention
Fig. 1 is high-activity crystal seed grain-size graph.
Fig. 2 is 1 product cut size figure of the embodiment of the present invention.
Fig. 3 is 1 product TGA of embodiment of the present invention figure.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples, and embodiment is not construed as limiting the scope of the present invention.
Embodiment 1
(1) sodium aluminate solution that 600mL has been handled well is added in the reactor, AO content is 255g/L, and α k is 1.47,
Heating stirring is slowly added to 60% nitric acid solution when temperature is stablized at 40 DEG C, and control reaction end pH is reacted 9 or so
After 1h, separation, washing, mashing obtain the high-activity crystal seed for being contained in 200g/L admittedly, crystal seed partial size (D50) it is 0.68 μm.
(2) the processed sodium aluminate solution of 1L is added in the reactor, AO content is 122g/L, and α k is 1.43, heating
Stirring is added at one time above-mentioned high-activity crystal seed when temperature is stablized at 70 DEG C, and seed is than controlling 2.5%, after reacting 10h,
Filtering, washing obtain aluminum hydroxide filter cake.
(3) after the mashing of above-mentioned aluminum hydroxide filter cake, 4% 2mol/L ammonium dihydrogen phosphate is added and is modified, is passed through after modified
Final aluminum hydroxide product is made in drying.Product cut size (D50) it is 1.841 μm, 5% weightless temperature of product is at 276.8 DEG C, oil suction
Rate is in 24g/100g linseed oil, and conductivity is in 22us/cm.
Fig. 1 show high-activity crystal seed grain-size graph.
Fig. 2 show the present embodiment product cut size figure.
Fig. 3 show the present embodiment product TGA figure.
Embodiment 2
(1) sodium aluminate solution that 600mL has been handled well is added in the reactor, AO content is 305g/L, and α k is 1.45,
Heating stirring is slowly added to 50% nitric acid solution when temperature is stablized at 45 DEG C, controls reaction end pH 8.5 or so, instead
After answering 1h, separation, washing, mashing obtain the high-activity crystal seed for being contained in 200g/L admittedly, crystal seed partial size (D50) it is 0.75 μm.
(2) the processed sodium aluminate solution of 1L is added in the reactor, AO content is 125g/L, and α k is 1.45, heating
Stirring is added at one time above-mentioned high-activity crystal seed when temperature is stablized at 72 DEG C, and seed is than controlling 1.5%, after reacting 8h,
Filtering, washing obtain aluminum hydroxide filter cake.
(3) after the mashing of above-mentioned aluminum hydroxide filter cake, 3% 2mol/L phosphoric acid is added and is modified, is made after modified through dry
Obtain final aluminum hydroxide product.Product cut size (D50) it is 2.185 μm, at 276.5 DEG C, oil absorbency exists 5% weightless temperature of product
25g/100g linseed oil, conductivity is in 20us/cm.
Embodiment 3
(1) sodium aluminate solution that 600mL has been handled well is added in the reactor, AO content is 205g/L, and α k is 1.4,
Heating stirring is slowly added to 85% glacial acetic acid solution when temperature is stablized at 55 DEG C, control reaction end pH 8.5 or so,
After reacting 1.5h, separation, washing, mashing obtain the high-activity crystal seed for being contained in 200g/L admittedly, crystal seed partial size (D50) it is 0.85 μm.
(2) the processed sodium aluminate solution of 1L is added in the reactor, AO content is 127g/L, and α k is 1.48, heating
When temperature is stablized at 68 DEG C above-mentioned high-activity crystal seed is added, seed is always than control in stirring when reaction starts and reacts 2h respectively
System is 3%, after reacting 10h, filters, and washing obtains aluminum hydroxide filter cake.
(3) after the mashing of above-mentioned aluminum hydroxide filter cake, 4% 1mol/L polyacrylic acid is added and is modified, it is modified after through dry
It is dry that final aluminum hydroxide product is made.Product cut size (D50) it is 3.203 μm, at 278 DEG C, oil absorbency exists 5% weightless temperature of product
22g/100g linseed oil, conductivity is in 18us/cm.
Embodiment 4
(1) sodium aluminate solution that 600mL has been handled well is added in the reactor, AO content is 297g/L, and α k is 1.31,
Heating stirring is slowly added to 40% sulfuric acid solution when temperature is stablized at 50 DEG C, and control reaction end pH is reacted 8 or so
After 0.5h, separation, washing, mashing obtain the high-activity crystal seed for being contained in 200g/L admittedly, crystal seed partial size (D50) it is 0.9 μm.
(2) the processed sodium aluminate solution of 1L is added in the reactor, AO content is 128g/L, and α k is 1.48, heating
Above-mentioned high-activity crystal seed, seed ratio is added when reaction starts and reacts 1h, 2h respectively when temperature is stablized at 70 DEG C in stirring
Control is 4%, after reacting 12h, filters, and washing obtains aluminum hydroxide filter cake.
(3) after above-mentioned aluminum hydroxide filter cake mashing, 5% 2mol/L phosphoric acid is added and the mixture of ammonium dihydrogen phosphate carries out
It is modified, final aluminum hydroxide product is made through drying after being modified.Product cut size (D50) it is 3.802 μm, 5% weightless temperature of product exists
279 DEG C, oil absorbency is in 20g/100g linseed oil, and conductivity is in 17us/cm.
Embodiment 5
(1) sodium aluminate solution that 600mL has been handled well is added in the reactor, AO content is 270g/L, and α k is 1.48,
Heating stirring is slowly added to 65% nitric acid solution when temperature is stablized at 35 DEG C, and control reaction end pH is reacted 9 or so
After 1h, separation, washing, mashing obtain the high-activity crystal seed for being contained in 200g/L admittedly, crystal seed partial size (D50) it is 0.69 μm.
(2) the processed sodium aluminate solution of 1L is added in the reactor, AO content is 125g/L, and α k is 1.5, and heating is stirred
Mix, when temperature is stablized at 70 DEG C, start respectively in reaction and when reaction 2h, 4h is added above-mentioned high-activity crystal seed, seed always than
Control is 3%, after reacting 12h, filters, and washing obtains aluminum hydroxide filter cake.
(3) after the mashing of above-mentioned aluminum hydroxide filter cake, 4% 2mol/L ammonium dihydrogen phosphate is added and is modified, is passed through after modified
Final aluminum hydroxide product is made in drying.Product cut size (D50) it is 3.203 μm, 5% weightless temperature of product is at 276 DEG C, oil absorbency
In 18g/100g linseed oil, conductivity is in 15us/cm.
Embodiment 1-5 prepares product index and existing products in markets index contrast table
Found out by above-mentioned data, embodiment 1-5 prepares product cut size (D50) between 1.5-5 μm, 5% weightless temperature exists
Between 275-280 DEG C, oil absorbency in 15-30g/100g linseed oil, conductivity in 10-30us/cm, can meet electronic circuit board or
The requirement of electrician trade.
Claims (10)
1. the preparation method of a kind of electronic circuit board or electrician's fire retardant aluminium hydroxide, which comprises the following steps:
(1) it is reacted using inorganic acid with sodium aluminate solution and prepares aluminium hydroxide crystal seed；
(2) crystal seed of step (1) preparation is added portionwise into sodium aluminate solution at 65-75 DEG C, is kept the temperature under stirring anti-
After answering 8-12h, filters pressing, washing obtain aluminum hydroxide filter cake；
(3) modifying agent is added after filter cake mashing to be modified, modified product is dried to obtain the hydroxide through drier
Aluminium product.
2. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In inorganic acid described in step (1) is any one of nitric acid, sulfuric acid or glacial acetic acid；The concentration wt% of the inorganic acid is 20-
95%；The AO content of the sodium aluminate solution is 200-350g/L；The process conditions of the reaction are as follows: 35-55 DEG C of temperature, reaction
The pH of terminal is 8-10, and reaction time 0.5-2h, product cut size is 0.6-1 μm.
3. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In inorganic acid described in step (1) is nitric acid, and concentration wt% is 40-65%；The AO content of the sodium aluminate solution is 240-
260g/L；The process conditions of the reaction are as follows: 40-50 DEG C of temperature, the pH of reaction end is 8-9, reaction time 1h.
4. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In the AO content of step (2) described sodium aluminate solution is 120-130g/L.
5. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In, be added portionwise the crystal seeds to divide 1-4 crowd that step (1) preparation is added described in step (2), the time of addition at the beginning of reaction extremely
It reacts between 4h, seed is always than controlling in 1-5%.
6. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In the crystal seed that step (1) preparation is added for point 1 batch or 3 batches being added portionwise described in step (2), the time of addition is reacting her
Begin between reaction 4h, seed is always than controlling in 1.5-3.5%.
7. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In modifying agent described in step (3) is one or more of phosphoric acid, polyacrylic acid, ammonium dihydrogen phosphate；The modifying agent adds
Dosage is 2-7%.
8. the preparation method of electronic circuit board according to claim 1 or electrician's fire retardant aluminium hydroxide, feature exist
In modifying agent described in step (3) is ammonium dihydrogen phosphate；Its additive amount is 3-5%.
9. the alumina fire retardant of the described in any item preparation method preparations of claim 1-10, which is characterized in that product cut size
D50It is 1.5-5 μm, 5% weightless temperature of product is 275-280 DEG C, and oil absorbency is 15-30g/100g linseed oil, conductivity 10-
30us/cm。
10. application of the alumina fire retardant as claimed in claim 9 in electronic circuit board or electrician trade.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099645A (en) * | 2019-12-23 | 2020-05-05 | 山东泰星新材料股份有限公司 | Preparation method of flower-shaped aluminum hydroxide for pouring sealant |
| CN111348667A (en) * | 2020-03-17 | 2020-06-30 | 山东省化工研究院 | High-activity monodisperse aluminum hydroxide seed crystal synthesis method |
| CN116216755A (en) * | 2023-01-31 | 2023-06-06 | 中铝山东有限公司 | Preparation method of low oil absorption micro powder aluminum hydroxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099645A (en) * | 2019-12-23 | 2020-05-05 | 山东泰星新材料股份有限公司 | Preparation method of flower-shaped aluminum hydroxide for pouring sealant |
| CN111099645B (en) * | 2019-12-23 | 2022-10-18 | 山东泰星新材料股份有限公司 | Preparation method of flower-shaped aluminum hydroxide for pouring sealant |
| CN111348667A (en) * | 2020-03-17 | 2020-06-30 | 山东省化工研究院 | High-activity monodisperse aluminum hydroxide seed crystal synthesis method |
| CN116216755A (en) * | 2023-01-31 | 2023-06-06 | 中铝山东有限公司 | Preparation method of low oil absorption micro powder aluminum hydroxide |
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Application publication date: 20191025 |
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