CN106977664A - A kind of preparation technology of high white superfine aluminium hydroxide dispersant special - Google Patents
A kind of preparation technology of high white superfine aluminium hydroxide dispersant special Download PDFInfo
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- CN106977664A CN106977664A CN201710280416.7A CN201710280416A CN106977664A CN 106977664 A CN106977664 A CN 106977664A CN 201710280416 A CN201710280416 A CN 201710280416A CN 106977664 A CN106977664 A CN 106977664A
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- aluminium hydroxide
- preparation technology
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- superfine aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
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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
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/16—Amines or polyamines
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
A kind of preparation technology of high white superfine aluminium hydroxide dispersant special, there is provided a kind of preparation technology of the dispersant needed for high white superfine aluminium hydroxide production process, polyether macromonomer is included using raw material, unsaturated carboxylic acid, polymerization inhibitor, acrylamide, chain-transferring agent, initiator, retarder, buffer, brightening agent and pH adjusting agent, by reacting polyether macromonomer organic synthesis polycarboxylic acids control in the course of the polymerization process, the polyocarboxy acid type macromolecule dispersing agent synthesized, dispersant whitening effect is good, the characteristics of raw material gloss can be improved, and there is preferable peptizaiton to slurry, addition is few during use, non-foam, high solid phase can be obtained under low viscosity, water-reducing rate is high；With good stability, substantially, dispersibility is protruded anti-settling effect；Addition can improve the suspension stability of slurry in process of lapping, improve the grinding effect of abrasive media；It is good with most of releasing agent compatibilities, do not reacted with mould, release property is good.
Description
Technical field
The invention belongs to chemical technology field, disperseing needed for specially a kind of high white superfine aluminium hydroxide production process
The preparation technology of agent.
Background technology
Aluminium hydroxide is a kind of conventional chemical addition agent, be widely used in fire-retardant, abrasive material, ceramics, industrial adsorbents and
Each field such as catalytic carrier, the quality of aluminium hydroxide also directly decides the quality of its product, aluminium-hydroxide powder particle diameter it is big
The small certain effects for affecting product.
The conventional ultrafine aluminium hydroxide particle diameter in current domestic and international market is generally 0.5 micron to 3 microns, being generally of production technology
Method, product cut size is more homogeneous, and purity performance is good, but cost is higher, complex process, needs to add dispersant in technical process
To realize its effect needed.Existing dispersant is generally the inorganic salts such as sodium carbonate, waterglass, sodium tripolyphosphate and organic small
Dispersal agent molecule, its stability and diminishing grinding-aid effect are all not ideal enough, are even more to be difficult to completely when tackling higher and higher require
Sufficient demand, it is therefore desirable to inquire into new dispersant to tackle industrial demand.
The content of the invention
It is an object of the invention to provide a kind of preparation technology of high white superfine aluminium hydroxide dispersant special, with solution
State problem.
To achieve the above object, technical scheme proposed by the present invention is：
A kind of preparation technology of high white superfine aluminium hydroxide dispersant special, it uses raw material to include polyether macromonomer, unsaturation
Carboxylic acid, polymerization inhibitor, acrylamide, chain-transferring agent, initiator, retarder, buffer, pH adjusting agent and brightening agent.
Technological process based on above-mentioned raw materials, be specially：
1. polyether macromonomer and appropriate amount of deionized water are added in four-hole boiling flask, opening mechanical agitation and heating makes polyether macromonomer
All dissolving, initiator is added in flask, stirred, mixture I is made, and be warming up to 50 ~ 100 DEG C with standby；
2. unsaturated carboxylic acid, acrylamide, chain-transferring agent and appropriate amount of deionized water are mixed into solution, are used as mixtures II；
3. the mixture I that mixtures II is added drop-wise in flask is reacted by constant pressure funnel, the follow-up continuation of insurance temperature 2 of completion of dropwise addition
To reacting complete, polymerization inhibitor is then added, stir cooling within ~ 6h hours；
4. after temperature is cooled to room temperature, add appropriate amount of deionized water, buffer, pH adjusting agent regulation solution in solid content and
PH, obtains solid content in polyocarboxy acid type macromolecule dispersing agent mother liquor, mother liquor and is adjusted to 6 ~ 8 more than 40%, pH；
5. retarder is added into mother liquor to be modified, and is added brightening agent and is stirred, that is, obtains to ultrafine aluminium hydroxide
Rise brighten, the polycarboxylic acids water-soluble polymer dispersant of peptizaiton：High white superfine aluminium hydroxide dispersant special.
In above-mentioned flow, unsaturated carboxylic acid consumption is the 15 ~ 50% of polyether macromonomer quality, and polymerization inhibitor consumption is polyethers
The 0.01 ~ 5% of polymeric monomer quality, acrylamide consumption is the 1 ~ 5% of polyether macromonomer quality, and chain-transferring agent consumption is the big list of polyethers
The 1 ~ 5% of weight, initiator amount is the 1 ~ 5% of polyether macromonomer quality, and retarder consumption is the 0.1 of dispersant mother liquor quality
~ 0.5%, buffer consumption be polyether macromonomer quality 0.01 ~ 5%, brightening agent consumption for dispersant mother liquor quality 0.1 ~
10%。
In the present invention, the polyether macromonomer is allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isoamyl
One or more of mixtures in alkenyl APEO.
In the present invention, the unsaturated carboxylic acid is itaconic acid, acrylic acid, methacrylic acid, butene dioic acid, maleic two
One or more of mixtures in acid anhydrides.
In the present invention, the polymerization inhibitor is polyatomic phenol, specially methyl hydroquinone, bisphenol-A, hydroquinones, right
One or more of mixtures in tert-butyl catechol.
In the present invention, the chain-transferring agent is one kind in 2 mercapto ethanol, TGA, mercaptopropionic acid, isopropanol
Or several mixtures.
In the present invention, the initiator be it is a kind of in potassium sulfate, ammonium persulfate, sodium peroxydisulfate, benzoyl peroxide or
Several and L-AA is mixed.
In the present invention, the retarder be citric acid, gluconic acid, salicylic salt, one kind in sugar derivatives or
Several mixtures.
In the present invention, the buffer is one or more of in calgon, sodium tripolyphosphate, sodium pyrophosphate
Mixture.
In the present invention, the pH adjusting agent is the not metal ion such as ethanol ammonium, diethanol ammonium, triethanol ammonium, ammoniacal liquor
Alkaline matter in one or more of mixtures.
In the present invention, the brightening agent is polyalcohol CX-CHO, the specially neighbour such as pentaerythrite, ethylene glycol, propane diols
One or more of mixtures in the polyalcohol of position.
In the present invention, because polyocarboxy acid type macromolecule dispersing agent mother liquor molecular structure is in pectination, side chain is more and long, molecule
Absorption is in slurry particle surface, and side chain stretches into liquid phase, and because its side chain is longer, adsorption layer is overlapped, forms huge three-dimensional suction
Attached structure, effectively prevents slurry particle aggregation, so that there is significant space steric effect between slurry particle, meanwhile, side
The hydrophilic active group also carried on chain（Such as-OH ,-O- ,-COO-）Associated in the form of hydrogen bond, in slurry particle surface
One layer of stabilization, hydrophily solid protective membrane with certain mechanical strength are formed, the film moistens slurry particle, and is easy to sliding
It is dynamic, not only with dispersiveness but also there is provided the dispersion stabilization of slurry particle.
For this dispersant, appropriate polymer molecular weight is the key for controlling dispersant effect, molecular weight mistake
It is high or too low larger on dispersive property influence, and the consumption of chain-transferring agent, initiator can significantly adjust molecular weight and intrinsic viscosity；
The reaction temperature of preparation process also has large effect to polymer molecular weight, and temperature is too high, reacts excessively violent, is easily formed
The excessive polymer of molecular weight, temperature is too low then to react slow, easily forms the less polymer of molecular weight.
Compared with prior art, the dispersant that preparation preparation technology of the invention is produced has that whitening effect is good, can change
The characteristics of kind raw material gloss, and the characteristics of have preferable peptizaiton to slurry, the advantage possessed has：Addition is few, still
High solid phase can be obtained under foam, low viscosity, water-reducing rate is high；With good stability, anti-settling effect substantially, dash forward by dispersibility
Go out；Small are influenceed on final products dielectric properties；The flow leveling of improvement system, improves tinting strength, tinting power and gloss；In process of lapping
Addition can improve the suspension stability of slurry, improve the grinding effect of abrasive media；It is good with most of releasing agent compatibilities, not with
Mould reacts, and release property is good.
Embodiment
Below in conjunction with specific preferred embodiment, the invention will be further described, but not thereby limiting the invention
Protection domain.
Case study on implementation 1：
Weigh allyl polyethenoxy ether 100g to add in four-hole boiling flask, addition deionized water stirring makes it all dissolve, added
Sodium peroxydisulfate 5g, stirs, and mixture I is made, and be warming up to 50 ~ 100 DEG C with standby；By acrylic acid 40g, acrylamide
3g, mercaptopropionic acid 5g are added in deionized water and are stirred mixed dissolution, are used as mixtures II；Mixtures II is added drop-wise to mixture again
Reacted in I, continue to keep 5h after completion of dropwise addition, add hydroquinones 3g, stir cooling, is cooled to room temperature, add
Solid content and pH in deionized water, calgon 3g, ammoniacal liquor regulation solution, obtain polyocarboxy acid type macromolecule dispersing agent female
Solid content is adjusted to 7 more than 40%, pH in 250 ~ 300g of liquid, mother liquor；Sodium salicylate 1g is added into mother liquor to be modified, then
Ethylene glycol 5g is added, is uniformly mixed and can obtain product dispersant.
Case study on implementation 2：
Weigh allyl polyethenoxy ether 50g and methyl allyl polyoxyethylene ether 50g to add in four-hole boiling flask, add deionization
Water is stirred, and its is all dissolved, and is added potassium peroxydisulfate 4g, is stirred, is made mixture I, and be warming up to 50 ~ 100 DEG C in case
With；Methacrylic acid 20g, acrylamide 4g, butene dioic acid 15g, isopropanol 3g are added in deionized water and stir mixed dissolution,
It is used as mixtures II；Mixtures II is added drop-wise in mixture I again and reacted, continues to keep 5h after completion of dropwise addition, is added double
Phenol A 3g, stir cooling, is cooled to room temperature, adds consolidating in deionized water, sodium tripolyphosphate 5g, ethanol ammonium regulation solution
State content and pH, obtain solid content in polyocarboxy acid type macromolecule dispersing agent 250 ~ 300g of mother liquor, mother liquor and are adjusted more than 40%, pH
For 7；Sodium citrate 1.2g is added into mother liquor to be modified, and is added propane diols 6g, is uniformly mixed and can obtain product
Dispersant.
Case study on implementation 3：
Weigh isopentene group APEO 100g to add in four-hole boiling flask, addition deionized water stirring makes it all dissolve, plus
Enter ammonium persulfate 5g, stir, mixture I is made, and be warming up to 50 ~ 100 DEG C with standby；By itaconic acid 30g, acrylic acid
20g, acrylamide 3g, TGA 4g are added in deionized water and are stirred mixed dissolution, are used as mixtures II；Again by mixtures II
It is added drop-wise in mixture I and is reacted, continues to keep 5h after completion of dropwise addition, add methyl hydroquinone 4g, stir cooling,
Room temperature is cooled to, the solid content and pH added in deionized water, sodium pyrophosphate 5g, ammoniacal liquor regulation solution obtains polyocarboxy acid type
Solid content is adjusted to 7 more than 40%, pH in macromolecule dispersing agent 250 ~ 300g of mother liquor, mother liquor；Gluconic acid is added into mother liquor
Sodium 1g is modified, and adds pentaerythrite 8g, is uniformly mixed and be can obtain product dispersant.
To sum up, the dispersant addition that preparation technology of the invention is produced is few, only 0.2% or so of slurry, still
High solid phase can be obtained under foam, low viscosity, water-reducing rate is high, with good stability, anti-settling effect substantially, dash forward by dispersibility
Go out, effect is notable.
Claims (10)
1. a kind of preparation technology of high white superfine aluminium hydroxide dispersant special, it is characterised in that it uses raw material to include polyethers
Polymeric monomer, unsaturated carboxylic acid, polymerization inhibitor, acrylamide, chain-transferring agent, initiator, retarder and pH adjusting agent,
Technological process based on above-mentioned raw materials, be specially：
1. polyether macromonomer and appropriate amount of deionized water are added in four-hole boiling flask, opening mechanical agitation and heating makes polyether macromonomer
All dissolving, initiator is added in flask, stirred, mixture I is made, and be warming up to 50 ~ 100 DEG C with standby；
2. unsaturated carboxylic acid, acrylamide, chain-transferring agent and appropriate amount of deionized water are mixed into solution, are used as mixtures II；
3. the mixture I that mixtures II is added drop-wise in flask is reacted by constant pressure funnel, the follow-up continuation of insurance temperature 2 of completion of dropwise addition
To reacting complete, polymerization inhibitor is then added, stir cooling within ~ 6h hours；
4. after temperature is cooled to room temperature, add appropriate amount of deionized water, buffer, pH adjusting agent regulation solution in solid content and
PH, obtains solid content in polyocarboxy acid type macromolecule dispersing agent mother liquor, mother liquor and is adjusted to 6 ~ 8 more than 40%, pH；
5. retarder is added into mother liquor to be modified, and is added brightening agent and is stirred, that is, obtains product dispersant；
Wherein：Unsaturated carboxylic acid consumption is the 15 ~ 50% of polyether macromonomer quality, and polymerization inhibitor consumption is polyether macromonomer quality
0.01 ~ 5%, acrylamide consumption be polyether macromonomer quality 1 ~ 5%, chain-transferring agent consumption for polyether macromonomer quality 1 ~
5%, initiator amount is the 1 ~ 5% of polyether macromonomer quality, and retarder consumption is the 0.1 ~ 0.5% of dispersant mother liquor quality, buffering
Agent consumption is the 0.01 ~ 5% of polyether macromonomer quality, and brightening agent consumption is the 0.1 ~ 10% of dispersant mother liquor quality.
2. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
Polyether macromonomer is one kind in allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isopentene group APEO
Or several mixtures.
3. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
Unsaturated carboxylic acid is one or more of mixed in itaconic acid, acrylic acid, methacrylic acid, butene dioic acid, maleic anhydride
Compound.
4. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
Polymerization inhibitor is polyatomic phenol, specially one kind in methyl hydroquinone, bisphenol-A, hydroquinones, p-tert-Butylcatechol or
Several mixtures.
5. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
Chain-transferring agent is one or more of mixtures in 2 mercapto ethanol, TGA, mercaptopropionic acid, isopropanol.
6. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
Initiator is one or more of and L-AA mixing in potassium sulfate, ammonium persulfate, sodium peroxydisulfate, benzoyl peroxide
Into.
7. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
Retarder is one or more of mixtures in citric acid, gluconic acid, salicylic salt, sugar derivatives.
8. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that buffering
Agent is one or more of mixtures in calgon, sodium tripolyphosphate, sodium pyrophosphate.
9. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that described
PH adjusting agent is the one or more in ethanol ammonium, diethanol ammonium, triethanol ammonium, ammoniacal liquor etc. the not alkaline matter of metal ion
Mixture.
10. the preparation technology of high white superfine aluminium hydroxide dispersant special according to claim 1, it is characterised in that institute
Brightening agent is stated for polyalcohol, specially one or more of mixing in the polyalcohol of the ortho position such as pentaerythrite, ethylene glycol, propane diols
Thing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111116837A (en) * | 2019-12-30 | 2020-05-08 | 上海东升新材料有限公司 | Efficient coarse whiting grinding dispersant with auxiliary whitening effect and preparation method thereof |
| CN111748184A (en) * | 2020-07-21 | 2020-10-09 | 苏州环诺新材料科技有限公司 | Fully-degradable high-fluidity PLA composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116837A (en) * | 2019-12-30 | 2020-05-08 | 上海东升新材料有限公司 | Efficient coarse whiting grinding dispersant with auxiliary whitening effect and preparation method thereof |
| CN111748184A (en) * | 2020-07-21 | 2020-10-09 | 苏州环诺新材料科技有限公司 | Fully-degradable high-fluidity PLA composite material and preparation method thereof |
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