CN105176142B - A kind of method of modifying of aluminium hydroxide - Google Patents
A kind of method of modifying of aluminium hydroxide Download PDFInfo
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- CN105176142B CN105176142B CN201510541765.0A CN201510541765A CN105176142B CN 105176142 B CN105176142 B CN 105176142B CN 201510541765 A CN201510541765 A CN 201510541765A CN 105176142 B CN105176142 B CN 105176142B
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Abstract
The present invention relates to a kind of method of modifying of aluminium hydroxide, the aluminum hydroxide filter cake obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed, which adds, is made aluminum hydroxide slurry in hollander tub, it is pumped into modified groove, aminopropyl trimethoxysilane oligomer is added to Modified by Aluminum Hydroxide, modified aluminum hydroxide slurry is dried to obtain aluminium hydroxide micro powder.There is the characteristics of modified effect is good, modification liquid usage amount is few, safe compared with prior art.
Description
Technical field
The present invention relates to powder surface modification technical field, specifically a kind of method of modifying of aluminium hydroxide.
Background technology
Aluminium hydroxide fire retardant has fire-retardant, smoke elimination, filling three zones, can be widely applied to the fire-retardant of high polymer material
And filling.Because aluminium hydroxide polarity is larger, and the influence of hydrogen bond, make easily to reunite between its particle；And aluminium hydroxide with
Organic polymer poor compatibility between the two, if being directly mixed with flame-proof composite material, it will disperse in the composite and point
Cloth is uneven, and larger particle diameter can also cause the stress concentration of composite, turn into the weak link of composite property, fill out
The big easy processing characteristics and mechanical property for influenceing composite of charge.So as to limit filler in the composite
Addition, product properties is had a strong impact on.Therefore must adopt an effective measure to improve the surface nature of aluminium hydroxide powder.
At present, typically using dry method modification and wet-process modified when surface is modified, dry method modification operating procedure is simple, but its
Modified cladding is uneven, clad ratio is low, and can produce substantial amounts of dust in process of production, causes the pollution of work-yard,
Form occupational disease risk hidden danger.In addition, dry method modification process, aluminium hydroxide micro powder is exposed to time length in open environment, also needs
Secondary package is carried out, it is easily contaminated.
Solve the problems, such as that dry method modification is present by wet-process modified, and modified effect is good, and silane idol is commonly used
Connection agent is modified, because common silane coupler is not soluble in water, so needing to add emulsifying agent progress in wet-process modified
Emulsification, silane coupler is relatively uniform after emulsification is dispersed in water, and strengthens modified effect, but even in wet-process modified middle silane
The unstability of hydrolysis be present, it is necessary to consume significant component of amount, therefore increase the use of modification liquid in the modification liquid for joining agent
Amount, also cause modifying agent and emulsifying agent solids residual excess to be present in aluminium hydroxide micro powder product, influence product purity.
The content of the invention
The present invention proposes a kind of method of modifying of aluminium hydroxide.
The technical proposal of the invention is realized in this way：A kind of method of modifying of aluminium hydroxide, it is characterised in that including step
Suddenly：
1）Mashing
The aluminum hydroxide filter cake obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed is added in hollander tub
Aluminum hydroxide slurry is made；
2）It is modified
By step 1）Obtained aluminum hydroxide slurry is pumped into modified groove, and adds aminopropyl trimethoxysilane oligomer
To Modified by Aluminum Hydroxide；
3）Drying
Modified aluminum hydroxide slurry is dried, obtains aluminium hydroxide micro powder.
As preferable technical scheme, the aminopropyl trimethoxysilane oligomer is by N-2- aminoethyl -3- aminopropyls
Trimethoxy silane hydrolytie polycondensation is made.
As preferable technical scheme, N-2- aminoethyl -3- aminopropyl trimethoxysilanes prepare aminopropyl trimethoxy
The operating method of silane low polymer is：N-2- aminoethyl -3- aminopropyl trimethoxysilanes are added in methoxyl group isopropanol, then
Catalyst and water are added, is 50 DEG C -60 DEG C in temperature, rotating speed stirs 10h-15h under conditions of being 2000rpm-3000rpm and carried out
Hydrolysis, then vacuum dehydration, aminopropyl trimethoxysilane oligomer is made.
As preferable technical scheme, during aminopropyl trimethoxysilane oligomer is prepared, N-2- aminoethyls-
3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, catalyst and the percentage by weight of water addition are：N-2- aminoethyls -3-
Aminopropyl trimethoxysilane 40%-50%, methoxyl group isopropanol 40%-50%, catalyst 1%-5%, water 8%-16%.
As preferable technical scheme, described catalyst is acetic acid, dibutyl tin laurate, stannous octoate or two vinegar
Any one in sour dibutyl tin.
As preferable technical scheme, the addition of the aminopropyl trimethoxysilane oligomer is aluminium hydroxide weight
0.8%-1.5%.
As preferable technical scheme, described water content in aluminum hydroxide filter cake is 45%-55%.
As preferable technical scheme, described drying temperature is 90 DEG C -160 DEG C.
By adopting the above-described technical solution, the present invention has beneficial effect following prominent：
1st, aluminium hydroxide is modified by the use of aminopropyl trimethoxysilane oligomer as modification liquid, with common silane
Coupling agent compares, and property changes, and is dissolved in water and does not hydrolyze, avoids using emulsifying agent, both improved modified effect and production
Product purity, the partially modified liquid loss caused by modification liquid hydrolyzes can be avoided again, the usage amount of modification liquid is reduced, reduces into
This.
2nd, when preparing aminopropyl trimethoxysilane oligomer with N-2- aminoethyl -3- aminopropyl trimethoxysilanes,
Substantial amounts of methoxyl group is deviate from hydrolysis condensation reaction, reduces the disaster hidden-trouble in production process, improves the peace of operation
Overall coefficient.
3rd, wet-process modified to be modified between mashing and drying, modified effect is good, and operating procedure is simple, reduces very
Big cost, wet-process modified material are pipeline, will not produce dust, reduce pollution.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Embodiment 1
A kind of method of modifying of aluminium hydroxide is：
（One）Prepare modification liquid：By N-2- aminoethyl -3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, acetic acid and
Water is mixed by weight percentage：N-2- aminoethyl -3- aminopropyl trimethoxysilanes 40%, methoxyl group isopropanol 50%, vinegar
Acid 1%, water 9%, polycondensation is hydrolyzed in stirring 15h under conditions of temperature is 50 DEG C, rotating speed is 3000rpm, then vacuum dehydration,
Modification liquid aminopropyl trimethoxysilane oligomer is made；
（Two）To Modified by Aluminum Hydroxide：The moisture content obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed
Added for 46% aluminum hydroxide filter cake in hollander tub, be pumped into modified groove after aluminum hydroxide slurry is made, add step（One）Prepare
Aminopropyl trimethoxysilane oligomer modification liquid, to aluminium hydroxide micro powder be modified, aminopropyl trimethoxysilane oligomer
Addition be aluminium hydroxide weight 0.8%, modified aluminum hydroxide slurry is dried at a temperature of 100 DEG C, obtains hydrogen
Alumina powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 4.75g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 95%.
Embodiment 2
A kind of method of modifying of aluminium hydroxide is：
（One）Prepare modification liquid：N-2- aminoethyl -3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, octanoic acid is sub-
Tin and water are mixed by weight percentage：N-2- aminoethyl -3- aminopropyl trimethoxysilanes 41%, methoxyl group isopropanol
42%, stannous octoate 1%, water 16%, polycondensation is hydrolyzed in stirring 13h under conditions of temperature is 55 DEG C, rotating speed is 2500rpm, so
Vacuum dehydration afterwards, modification liquid aminopropyl trimethoxysilane oligomer is made；
（Two）To Modified by Aluminum Hydroxide：The moisture content obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed
Added for 45% aluminum hydroxide filter cake in hollander tub, add step（One）The aminopropyl trimethoxysilane oligomer of preparation changes
Property liquid, aluminium hydroxide micro powder is modified, the addition of aminopropyl trimethoxysilane oligomer is the 0.9% of aluminium hydroxide weight,
Modified aluminum hydroxide slurry is dried at a temperature of 160 DEG C, obtains aluminium hydroxide micro powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 4.65g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 93%.
Embodiment 3
A kind of method of modifying of aluminium hydroxide is：
（One）Prepare modification liquid：By N-2- aminoethyl -3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, two bays
Sour dibutyl tin and water are mixed by weight percentage：N-2- aminoethyl -3- aminopropyl trimethoxysilanes 50%, methoxyl group
Isopropanol 40%, dibutyl tin laurate 2%, water 8%, stirring 10h enters under conditions of temperature is 60 DEG C, rotating speed is 2000rpm
Row hydrolytie polycondensation, then vacuum dehydration, modification liquid aminopropyl trimethoxysilane oligomer is made；
（Two）To Modified by Aluminum Hydroxide：By the hydroxide that the moisture content obtained after aluminium hydroxide micro powder slurries press filtration is 55%
Aluminium filter cake is added in hollander tub, and step is added in pulping process（One）The aminopropyl trimethoxysilane oligomer of preparation is modified
Liquid, aluminium hydroxide micro powder is modified, the addition of aminopropyl trimethoxysilane oligomer is the 1.5% of aluminium hydroxide weight, will
Modified aluminum hydroxide slurry is dried at a temperature of 90 DEG C, obtains aluminium hydroxide micro powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 4.83g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 96.6%.
Embodiment 4
A kind of method of modifying of aluminium hydroxide is：
（One）Prepare modification liquid：By N-2- aminoethyl -3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, two acetic acid
Dibutyl tin and water are mixed by weight percentage：N-2- aminoethyl -3- aminopropyl trimethoxysilanes 40%, methoxyl group is different
Propyl alcohol 45%, dibutyltin diacetate 5%, water 10%, 12h progress is stirred under conditions of temperature is 57 DEG C, rotating speed is 2200rpm
Hydrolytie polycondensation, then vacuum dehydration, modification liquid aminopropyl trimethoxysilane oligomer is made；
（Two）To Modified by Aluminum Hydroxide：The moisture content obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed
Added for 50% aluminum hydroxide filter cake in hollander tub, add step（One）The aminopropyl trimethoxysilane oligomer of preparation changes
Property liquid, aluminium hydroxide micro powder is modified, the addition of aminopropyl trimethoxysilane oligomer is the 1.2% of aluminium hydroxide weight,
Modified aluminum hydroxide slurry is dried at a temperature of 120 DEG C, obtains aluminium hydroxide micro powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 4.76g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 95.2%.
Embodiment 5
A kind of method of modifying of aluminium hydroxide is：
（One）Prepare modification liquid：By N-2- aminoethyl -3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, two acetic acid
Dibutyl tin and water are mixed by weight percentage：N-2- aminoethyl -3- aminopropyl trimethoxysilanes 42%, methoxyl group is different
Propyl alcohol 47%, dibutyltin diacetate 2%, water 9%, stirring 14h enters water-filling under conditions of temperature is 52 DEG C, rotating speed is 2700rpm
Polycondensation is solved, then vacuum dehydration, modification liquid aminopropyl trimethoxysilane oligomer is made；
（Two）To Modified by Aluminum Hydroxide：By the hydroxide that the moisture content obtained after aluminium hydroxide micro powder slurries press filtration is 48%
Aluminium filter cake is added in hollander tub, and step is added in pulping process（One）The aminopropyl trimethoxysilane oligomer of preparation is modified
Liquid, aluminium hydroxide micro powder is modified, the addition of aminopropyl trimethoxysilane oligomer is the 1.3% of aluminium hydroxide weight, will
Modified aluminum hydroxide slurry is dried at a temperature of 140 DEG C, obtains aluminium hydroxide micro powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 4.66g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 93.2%.
Comparative example 1
A kind of method of modifying of aluminium hydroxide is：
The aluminum hydroxide filter cake that the moisture content obtained after aluminium hydroxide micro powder slurries press filtration is 50% is added in hollander tub,
Weight is added in pulping process to be modified for the N-2- aminoethyl -3- aminopropyl trimethoxysilanes of aluminium hydroxide weight 1.2%
Liquid, aluminium hydroxide micro powder is modified, modified aluminum hydroxide slurry is dried at a temperature of 120 DEG C, obtains aluminium hydroxide
Micro mist.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 3.62g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 72.4%.
Comparative example 2
A kind of method of modifying of aluminium hydroxide is：
（One）Emulsifying agent stearic acid list glyceride is added in N-2- aminoethyl -3- aminopropyl trimethoxysilanes, to N-
2- aminoethyl -3- aminopropyl trimethoxysilanes are emulsified, and addition is N-2- aminoethyl -3- aminopropyl trimethoxysilanes
The 1% of weight；
（Two）The moisture content obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed is 50% aluminium hydroxide
Filter cake is added in hollander tub, adds step（One）N-2- aminoethyl -3- aminopropyl trimethoxysilanes after obtained emulsification change
Property liquid, aluminium hydroxide micro powder is modified, the weight of N-2- aminoethyl -3- aminopropyl trimethoxysilanes is hydrogen-oxygen after adding emulsification
Change aluminium weight 1.2%, modified aluminum hydroxide slurry is dried at a temperature of 120 DEG C, obtains aluminium hydroxide micro powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 3.76g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 75.2%.
Comparative example 3
A kind of method of modifying of aluminium hydroxide is：
（One）Emulsifying agent stearic acid list glyceride is added in N-2- aminoethyl -3- aminopropyl trimethoxysilanes, to N-
2- aminoethyl -3- aminopropyl trimethoxysilanes are emulsified, and addition is N-2- aminoethyl -3- aminopropyl trimethoxysilanes
The 1% of weight；
（Two）The moisture content obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed is 50% aluminium hydroxide
Filter cake is added in hollander tub, adds step（One）N-2- aminoethyl -3- aminopropyl trimethoxysilanes after obtained emulsification change
Property liquid, aluminium hydroxide micro powder is modified, the weight of N-2- aminoethyl -3- aminopropyl trimethoxysilanes is hydrogen-oxygen after adding emulsification
Change aluminium weight 2.8%, modified aluminum hydroxide slurry is dried at a temperature of 120 DEG C, obtains aluminium hydroxide micro powder.
Activation index determines：Take step（Two）The modified aluminium hydroxide micro powder 5g of gained, is placed in graduated cylinder, adds
100ml distilled water, vibration, standing, after stable system, pipette floating fraction on the water surface, dry, accurate weighing obtains 4.12g,
Activation index=floating quality (g)/sample quality (g).Calculate activation index be 82.4%.
In order to avoid once testing existing accidentalia, many experiments were done repeatedly, above-mentioned each group experimental data is
The experimental data wherein once tested, every group of experimental result is compared with the experimental result of other many experiments, and there was no significant difference
（P>0.05).
As a result：From the point of view of the activation index of comprehensive each embodiment group and each comparative example group, the activation index of five embodiment groups
It is higher, and the activation index between each embodiment group is compared to there was no significant difference（P>0.05), it can be verified that used herein
Aminopropyl trimethoxysilane oligomer modification liquid the modified effect to aluminium hydroxide micro powder it is preferable, and usage amount is smaller,
Cost is low；From the point of view of activation index as obtained by 3 groups of 1 group of comparative example, 2 groups of comparative example and comparative example, common silane coupler
The modified effect of modification liquid is poor, the silane coupler added after emulsifying agent, although changing the water solubility of silane coupler,
The usage amount of modification liquid is more, and cost is high, and modified effect is significantly lower than 4 groups of embodiment（P<0.05).
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (4)
1. a kind of method of modifying of aluminium hydroxide, it is characterised in that including step：
1) it is beaten
The aluminum hydroxide filter cake obtained after aluminium hydroxide micro powder and sodium aluminate hydraulic hybrid filtering are washed is added in hollander tub and is made
Aluminum hydroxide slurry；
2) it is modified
Aluminum hydroxide slurry made from step 1) is pumped into modified groove, and adds aminopropyl trimethoxysilane oligomer to hydrogen
It is alumina modified；The addition of the aminopropyl trimethoxysilane oligomer is the 0.8%-1.5% of aluminium hydroxide weight；Institute
State aminopropyl trimethoxysilane oligomer to be made by N-2- aminoethyl -3- aminopropyl trimethoxysilane hydrolytie polycondensations, operate
Method is：N-2- aminoethyl -3- aminopropyl trimethoxysilanes are added in methoxyl group isopropanol, add catalyst and water,
It it is 50 DEG C -60 DEG C in temperature, stirring 10h-15h is hydrolyzed under conditions of rotating speed is 2000rpm-3000rpm, and then vacuum takes off
Water, aminopropyl trimethoxysilane oligomer is made；The catalyst be acetic acid, dibutyl tin laurate, stannous octoate or
Any one in dibutyltin diacetate；
3) dry
Modified aluminum hydroxide slurry is dried, obtains aluminium hydroxide micro powder.
2. according to a kind of method of modifying of aluminium hydroxide described in claim 1, it is characterised in that：Preparing aminopropyl trimethoxy
During base silane oligomer, N-2- aminoethyl -3- aminopropyl trimethoxysilanes, methoxyl group isopropanol, catalyst and water
The percentage by weight of addition is：N-2- aminoethyls -3- aminopropyl trimethoxysilane 40%-50%, methoxyl group isopropanol 40%-
50%, catalyst 1%-5%, water 8%-16%.
3. according to a kind of method of modifying of aluminium hydroxide described in claim 1, it is characterised in that：Described aluminum hydroxide filter cake
Moisture content is 45%-55%.
4. according to a kind of method of modifying of aluminium hydroxide described in claim 1, it is characterised in that：Described drying temperature is 90
℃-160℃。
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| CN107416877A (en) * | 2017-05-12 | 2017-12-01 | 山东林嘉新材料科技有限公司 | The technique of organic matter, iron and silica in a kind of removing sodium aluminate solution |
| CN109054089A (en) * | 2018-06-27 | 2018-12-21 | 武宣宝丰矿业有限公司 | Active magnesium hydroxide fire retardants and preparation method thereof |
| CN109251397B (en) * | 2018-10-26 | 2021-01-12 | 安庆市悦发管业有限公司 | High-strength HDPE corrugated pipe material and preparation method thereof |
| CN109437268B (en) * | 2018-12-10 | 2021-02-19 | 贵州博汇联润铝业有限公司 | Method for improving activity of superfine and ultra-white aluminum hydroxide micro powder |
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|---|---|---|---|---|
| EP0307795A2 (en) * | 1987-09-14 | 1989-03-22 | MD Papier GmbH & Co. KG | Cationically modified pigmentary dispersion and coating colour |
| CN101134852A (en) * | 2007-10-15 | 2008-03-05 | 江苏河海纳米科技股份有限公司 | Inorganic powder organic surface modifying method |
| CN102634065A (en) * | 2012-04-26 | 2012-08-15 | 江苏达胜高聚物有限公司 | Preparation method of high-flame-retardant surface modified nano aluminum hydroxide |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0307795A2 (en) * | 1987-09-14 | 1989-03-22 | MD Papier GmbH & Co. KG | Cationically modified pigmentary dispersion and coating colour |
| CN101134852A (en) * | 2007-10-15 | 2008-03-05 | 江苏河海纳米科技股份有限公司 | Inorganic powder organic surface modifying method |
| CN102634065A (en) * | 2012-04-26 | 2012-08-15 | 江苏达胜高聚物有限公司 | Preparation method of high-flame-retardant surface modified nano aluminum hydroxide |
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