CN108409899A - A kind of cerium salt causes the preparation method of attapulgite/polyacrylic complex thickener - Google Patents
A kind of cerium salt causes the preparation method of attapulgite/polyacrylic complex thickener Download PDFInfo
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- CN108409899A CN108409899A CN201810118693.2A CN201810118693A CN108409899A CN 108409899 A CN108409899 A CN 108409899A CN 201810118693 A CN201810118693 A CN 201810118693A CN 108409899 A CN108409899 A CN 108409899A
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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
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C08F122/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides or nitriles thereof
- C08F122/02—Acids; Metal salts or ammonium salts thereof, e.g. maleic acid or itaconic acid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/43—Thickening agents
Abstract
The invention belongs to field of new materials, and in particular to a kind of cerium salt causes the preparation method of attapulgite/polyacrylic complex thickener, and this method utilizes the reproducibility and Ce of attapulgite's surface sulfydryl4+Strong oxidizing property constitute redox initiation system, use it for the initiation of acrylic monomer, by the way of inverse emulsion polymerization, prepare attapulgite/polyacrylic complex thickener, gained thickener thickening properties are excellent, and electrolyte resistance is good.
Description
Technical field
The invention belongs to field of new materials, and in particular to a kind of cerium salt initiation attapulgite/polyacrylic composite thickening
The preparation method of agent.
Background technology
Thickener is the important component of print paste.Agent for polyacrylic acid thickening thickening capabilities are strong, have a wide range of application；
But agent for polyacrylic acid thickening electrolyte-resistant ability is poor, and use cost is high.Attapulgite is a kind of porous type chain layered hydrous
Rich magnesium alumino metasilicate salt clay mineral, attapulgite is compound with agent for polyacrylic acid thickening, it can not only reduce polyacrylic
The production cost of thickener, and its electrolyte resistance can be improved.It is and organic however, attapulgite is a kind of inorganic material
Polymer compatibility is poor, how to realize that the combination of the two, the excellent attapulgite/polyacrylic of processability are compound
Thickener is always the direction that material supply section scholars make great efforts.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of cerium salts to cause the compound increasing of attapulgite/polyacrylic
Thick dose of preparation method, this method introduce sulfydryl in attapulgite's surface first, utilize the reproducibility and Ce of sulfydryl4+Strong oxdiative
Property constitute oxidization-reduction type cause system, use it for the initiation of acrylic monomer, by the way of inverse emulsion polymerization,
Prepare attapulgite/polyacrylic complex thickener.The good thixotropy of attapulgite is cooperateed with organic polymer thickener
Effect reaches mutual supplement with each other's advantages.
Realizing the technical solution of above-mentioned purpose is：A kind of cerium salt causes attapulgite/polyacrylic complex thickener
Preparation method is first modified attapulgite using silane coupling agent, its surface introduce sulfydryl, then with Ce4+It constitutes
Oxidation-reduction trigger system, the initiation for acrylic monomer polymerize.
A kind of cerium salt provided by the invention causes the preparation method of attapulgite/polyacrylic complex thickener, including
Following steps：
(1) by attapulgite with solid-liquid mass ratio 1:100-4:100 are scattered in organic solvent, ultrasonic disperse 30-
Silane coupling agent is added dropwise in 60min, and under nitrogen protection, stirring, heating reflux reaction 12-24h removes solvent after reaction,
Vacuum drying, grinding cross 200 mesh sieve to get sulfydryl attapulgite；
Wherein, organic solvent is toluene or dimethylbenzene；Silane coupling agent is 3- mercaptopropyl trimethoxysilanes or 3- mercaptos third
Ethyl triethoxy silicane alkane, silane coupling agent are 2 with attapulgite mass ratio:1-5:1；
(2) four-hole boiling flask is placed in cold bath, unsaturated acid monomer, sulfydryl attapulgite, sulfydryl concave convex rod is added
Soil accounts for the 20%-40% of unsaturated acid monomer mass, and ammonium hydroxide is slowly added dropwise to 6,500 revs/min of stirring 30- of solution ph
60min obtains aqueous-phase material；Emulsifier, crosslinking agent and organic solvent are made into oil phase, aqueous-phase material is added to oil phase under stirring condition
In, after 1000-1500 revs/min of high speed emulsification 60-90min, it is warming up to 50-60 DEG C, under 300-450 revs/min of stirring condition, drop
Add initiator solution, after completion of dropwise addition, is continuously heating to 60-70 DEG C, reacts 1-3h, after reaction, cooling discharging, then
Addition phase inversion agent, which stirs evenly, to get product.
Wherein, unsaturated acid monomer is acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, maleic anhydride
In one kind or arbitrary combination.
Wherein, mentioned emulsifier is sorbitan fatty acid ester or polyoxyethylene sorbitan fatty acid ester, emulsification
The dosage of agent accounts for the 2-8% of unsaturated acid monomer mass.
Above-mentioned crosslinking agent is diallyl phthalate, and crosslinking agent quality accounts for the 0.1%- of unsaturated acid monomer mass
0.25%.
Above-mentioned organic solvent is 120# gasoline, 200# gasoline, one kind in kerosene, 5# white oils, unsaturated acid monomer with
Organic solvent mass ratio 0.25:1-0.6:1.
Above-mentioned initiator is Cericammoniumsulfate or ammonium ceric nitrate, and initiator quality accounts for the 0.5%- of unsaturated acid monomer mass
1.0%.
Above-mentioned phase inversion agent is isomerous tridecanol polyoxyethylene ether or fatty alcohol polyoxyethylene ether, and dosage accounts for unsaturated acidity
The 4-6% of monomer mass.
The beneficial effects of the invention are as follows：Utilize the reproducibility and Ce of recessed native surface sulfydryl4+Strong oxidizing property constitute oxidation-also
Prototype causes system and causes polymerization, and attapulgite is good with organic polymer compatibility, gained thickener thickening properties, electrolyte-resistant
It has excellent performance.
Specific implementation mode
With reference to specific embodiment, description is of the invention in further detail.It should be understood that these embodiments are intended merely to
It illustrates the present invention, rather than limits the scope of the invention in any way.
Embodiment 1
(1) by attapulgite with solid-liquid mass ratio 1:100 are scattered in toluene, ultrasonic disperse 30min, and 3- mercapto propyl is added dropwise
Trimethoxy silane, 3- mercaptopropyl trimethoxysilanes are 2 with attapulgite mass ratio:1, it under nitrogen protection, stirs, heating
Back flow reaction 12h removes solvent after reaction, is dried in vacuo, grinding, crosses 200 mesh sieve to get sulfydryl attapulgite；
(2) four-hole boiling flask is placed in cold bath, acrylic acid, sulfydryl attapulgite is added, sulfydryl attapulgite accounts for propylene
The 20% of sour quality is slowly added dropwise ammonium hydroxide to 6,500 revs/min of stirring 30min of solution ph, obtains aqueous-phase material；By anhydrous sorbitol
Aliphatic ester, diallyl phthalate and 120# gasoline are made into oil phase, and the dosage of sorbitan fatty acid ester accounts for propylene
The 2% of sour quality, diallyl phthalate account for the 0.1% of acrylic acid quality, the ratio between acrylic acid and 120# qualities of gasoline
It is 0.25:1, aqueous-phase material is added into oil phase under stirring condition, after 1000 revs/min of high speed emulsification 90min, is warming up to 50 DEG C,
Under 300 revs/min of stirring conditions, initiator Cericammoniumsulfate aqueous solution is added dropwise, Cericammoniumsulfate quality accounts for acrylic acid quality
0.5%, after completion of dropwise addition, 60 DEG C are continuously heating to, reacts 3h, after reaction, then phase inversion agent isomery is added in cooling discharging
Tridecanol polyoxyethylene ether, dosage account for the 4% of acrylic acid quality, stir evenly and get product.
Comparative example 1
Four-hole boiling flask is placed in cold bath, acrylic acid, attapulgite is added, attapulgite accounts for acrylic acid quality
20%, ammonium hydroxide is slowly added dropwise to 6,500 revs/min of stirring 30min of solution ph, obtains aqueous-phase material；By sorbitan fatty acid ester,
Diallyl phthalate is made into oil phase with 120# gasoline, and the dosage of sorbitan fatty acid ester accounts for acrylic acid quality
2%, diallyl phthalate accounts for the 0.1% of acrylic acid quality, and the ratio between acrylic acid and 120# qualities of gasoline are 0.25:1,
Aqueous-phase material is added into oil phase under stirring condition, after 1000 revs/min of high speed emulsification 90min, 50 DEG C are warming up to, at 300 revs/min
Under stirring condition, initiator Cericammoniumsulfate aqueous solution is added dropwise, Cericammoniumsulfate quality accounts for the 0.5% of acrylic acid quality, completion of dropwise addition
Afterwards, 60 DEG C are continuously heating to, 3h is reacted, after reaction, then phase inversion agent isomerous tridecanol polyoxyethylene is added in cooling discharging
Ether, dosage account for the 4% of acrylic acid quality, stir evenly and get product.
Comparative example 2a
Four-hole boiling flask is placed in cold bath, acrylic acid, attapulgite is added, attapulgite accounts for acrylic acid quality
20%, ammonium hydroxide is slowly added dropwise to 6,500 revs/min of stirring 30min of solution ph, obtains aqueous-phase material；By sorbitan fatty acid ester,
Diallyl phthalate is made into oil phase with 120# gasoline, and the dosage of sorbitan fatty acid ester accounts for acrylic acid quality
2%, diallyl phthalate accounts for the 0.1% of acrylic acid quality, and the ratio between acrylic acid and 120# qualities of gasoline are 0.25:1,
Aqueous-phase material is added into oil phase under stirring condition, after 1000 revs/min of high speed emulsification 90min, 50 DEG C are warming up to, at 300 revs/min
Under stirring condition, initiator ammonium persulfate aqueous solution is added dropwise, ammonium persulfate quality accounts for the 0.5% of acrylic acid quality, completion of dropwise addition
Afterwards, 60 DEG C are continuously heating to, 3h is reacted, after reaction, then phase inversion agent isomerous tridecanol polyoxyethylene is added in cooling discharging
Ether, dosage account for the 4% of acrylic acid quality, stir evenly and get product.
Comparative example 2b
Four-hole boiling flask is placed in cold bath, acrylic acid is added, ammonium hydroxide is slowly added dropwise and is stirred for 6,500 revs/min to solution ph
30min is mixed, aqueous-phase material is obtained；Sorbitan fatty acid ester, diallyl phthalate and 120# gasoline are made into oil phase, lost
The dosage of water Span accounts for the 2% of acrylic acid quality, and diallyl phthalate accounts for acrylic acid quality
0.1%, the ratio between acrylic acid and 120# qualities of gasoline are 0.25:1, aqueous-phase material is added into oil phase under stirring condition, 1000
Rev/min high speed emulsification 90min after, be warming up to 50 DEG C, under 300 revs/min of stirring conditions, be added dropwise initiator ammonium persulfate it is water-soluble
Liquid, ammonium persulfate quality accounts for the 0.5% of acrylic acid quality, after completion of dropwise addition, is continuously heating to 60 DEG C, reacts 3h, reaction terminates
Afterwards, then phase inversion agent isomerous tridecanol polyoxyethylene ether is added in cooling discharging, dosage accounts for the 4% of acrylic acid quality, and stirring is equal
It is even to get product.
Embodiment 2
(1) by attapulgite with solid-liquid mass ratio 4:100 are scattered in dimethylbenzene, ultrasonic disperse 60min, and 3- mercaptos third are added dropwise
Ethyl triethoxy silicane alkane, 3- mercaptopropyltriethoxysilanes are 5 with attapulgite mass ratio:1, under nitrogen protection, stirring adds
Hot back flow reaction for 24 hours, after reaction, removes solvent, is dried in vacuo, grinding, crosses 200 mesh sieve to get sulfydryl attapulgite；
(2) four-hole boiling flask is placed in cold bath, methacrylic acid, sulfydryl attapulgite is added, sulfydryl attapulgite accounts for
The 40% of methacrylic acid quality is slowly added dropwise ammonium hydroxide to 6,500 revs/min of stirring 60min of solution ph, obtains aqueous-phase material；It will gather
Ethylene oxide sorbitan fatty acid ester, diallyl phthalate and 200# gasoline are made into oil phase, polyoxyethylene sorbitan mountain
Pears alcohol fatty acid ester accounts for the 8% of methacrylic acid quality, and diallyl phthalate quality accounts for methacrylic acid monomer quality
0.25%, the ratio between methacrylic acid and 200# quality of gasolines 0.6:1, aqueous-phase material is added into oil phase under stirring condition,
After 1500 revs/min of high speed emulsification 60min, 60 DEG C are warming up to, under 450 revs/min of stirring conditions, ammonium ceric nitrate aqueous solution is added dropwise,
Ammonium ceric nitrate quality accounts for the 1.0% of methacrylic acid monomer quality, after completion of dropwise addition, is continuously heating to 70 DEG C, reacts 1h, reaction
After, then fatty alcohol polyoxyethylene ether is added in cooling discharging, dosage accounts for the 6% of methacrylic acid monomer quality, stirring
Uniformly get product.
Embodiment 3
(1) by attapulgite with solid-liquid mass ratio 2:100 are scattered in toluene, ultrasonic disperse 40min, and 3- mercapto propyl is added dropwise
Trimethoxy silane, 3- mercaptopropyl trimethoxysilanes are 3 with attapulgite mass ratio:1, it under nitrogen protection, stirs, heating
Back flow reaction 16h removes solvent after reaction, is dried in vacuo, grinding, crosses 200 mesh sieve to get sulfydryl attapulgite；
(2) four-hole boiling flask is placed in cold bath, itaconic acid, sulfydryl attapulgite is added, sulfydryl attapulgite accounts for clothing health
The 30% of sour quality is slowly added dropwise ammonium hydroxide to 6,500 revs/min of stirring 40min of solution ph, obtains aqueous-phase material；By anhydrous sorbitol
Aliphatic ester, diallyl phthalate and kerosene are made into oil phase, and sorbitan fatty acid ester accounts for itaconic acid quality
4%, diallyl phthalate quality accounts for the 0.15% of itaconic acid quality, itaconic acid and kerosene mass ratio 0.4:1, stirring
Under the conditions of aqueous-phase material is added into oil phase, 1200 revs/min high speed emulsification 70min after, be warming up to 55 DEG C, at 350 revs/min stir
Under the conditions of, Cericammoniumsulfate aqueous solution is added dropwise, Cericammoniumsulfate quality accounts for the 0.6% of itaconic acid quality, after completion of dropwise addition, continues to heat up
To 65 DEG C, 2h is reacted, after reaction, then isomerous tridecanol polyoxyethylene ether is added in cooling discharging, dosage accounts for itaconic acid
The 5% of quality, stirs evenly and gets product.
Embodiment 4
(1) by attapulgite with solid-liquid mass ratio 3:100 are scattered in dimethylbenzene, ultrasonic disperse 50min, and 3- mercaptos third are added dropwise
Ethyl triethoxy silicane alkane, 3- mercaptopropyltriethoxysilanes are 4 with attapulgite mass ratio:1, under nitrogen protection, stirring adds
Hot back flow reaction 20h removes solvent after reaction, is dried in vacuo, grinding, crosses 200 mesh sieve to get sulfydryl attapulgite；
(2) four-hole boiling flask is placed in cold bath, fumaric acid, sulfydryl attapulgite is added, sulfydryl attapulgite accounts for rich horse
The 35% of sour quality is slowly added dropwise ammonium hydroxide to 6,500 revs/min of stirring 50min of solution ph, obtains aqueous-phase material；Polyoxyethylene is lost
Water Span, diallyl phthalate and 5# white oils are made into oil phase, polyoxyethylene sorbitan aliphatic acid
The dosage of ester accounts for the 6% of fumaric acid quality, and diallyl phthalate quality accounts for the 0.2% of fumaric acid quality, fumaric acid with
The ratio between 5# white oil qualities 0.5:1, aqueous-phase material is added into oil phase under stirring condition, after 1300 revs/min of high speed emulsification 80min,
58 DEG C are warming up to, under 400 revs/min of stirring conditions, ammonium ceric nitrate aqueous solution is added dropwise, ammonium ceric nitrate accounts for fumaric acid quality
0.8%, after completion of dropwise addition, 68 DEG C are continuously heating to, reacts 2.5h, after reaction, then poly alkyl alcohol is added in cooling discharging
Ethylene oxide ether, fatty alcohol polyoxyethylene ether quality account for the 5.5% of fumaric acid quality, stir evenly and get product.
Embodiment 5
It is accurate to weigh 2g thickeners, 98g distilled water is added, stirs and be added dropwise 3-4 drop ammonium hydroxide, is sufficiently stirred and is made into quality point
The white slurry of number 2%.It is surveyed at room temperature at constant rotational speed 10 revs/min (No. 6 rotors) with II+Pro viscosimeters of Brookfield DV-
The viscosity of ding white ware slurry.
Electrolyte resistance is indicated with viscosity retention ratio, is measured above-mentioned thickener and is starched addition 0.05%NaCl (solid) in vain in vain
Slurry viscosity, viscosity retention ratio=ηAfter adding NaCl/ηBefore adding NaCl, viscosity retention ratio is higher, and electrolyte-resistant is better.
1 sample thickening properties of table
As can be seen from the above table, thickener obtained by embodiment 1-4 has very strong thickening capabilities, and electrolyte resistance is excellent
It is different.In comparative example 1, since attapulgite is modified without mercaptosilane coupling agents, it is complete that Cericammoniumsulfate cannot cause acrylic monomers
Full polymerization, gained thickener thickening properties are very poor.Comparative example 2a causes monomer polymerization using traditional ammonium persulfate, and products obtained therefrom is most
Pipe thickening properties and electrolyte resistance are preferable, but still are slightly inferior to embodiment 1, it may be possible to since attapulgite is in polyacrylic acid
Caused by middle dispersion performance is bad.In comparative example 2b, due to being not added with attapulgite, products obtained therefrom thickening properties are less better, resistance to
Electrolyte performance is also very poor.
Claims (9)
1. a kind of cerium salt causes the preparation method of attapulgite/polyacrylic complex thickener, it is characterised in that：The side
Method is to introduce sulfydryl in attapulgite's surface first, utilize the reproducibility and Ce of sulfydryl4+Strong oxidizing property constitute oxidationreduction
Type causes system, uses it for the initiation of acrylic monomer, by the way of inverse emulsion polymerization, prepares attapulgite/poly-
Acrylic compounds complex thickener.
2. a kind of cerium salt as described in claim 1 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：The method the specific steps are,
(1) by attapulgite with solid-liquid mass ratio 1:100-4:100 are scattered in organic solvent, ultrasonic disperse 30-60min, drop
Adding silane coupling agent, under nitrogen protection, stirring, heating reflux reaction 12-24h removes solvent after reaction, vacuum drying,
Grinding crosses 200 mesh sieve to get sulfydryl attapulgite；
(2) four-hole boiling flask is placed in cold bath, unsaturated acid monomer, sulfydryl attapulgite is added, sulfydryl attapulgite accounts for
The 20%-40% of unsaturated acidity monomer mass is slowly added dropwise ammonium hydroxide to 6,500 revs/min of stirring 30-60min of solution ph, obtains
Aqueous-phase material；Emulsifier, crosslinking agent and organic solvent are made into oil phase, aqueous-phase material is added into oil phase under stirring condition, 1000-
After 1500 revs/min of high speed emulsification 60-90min, it is warming up to 50-60 DEG C, under 300-450 revs/min of stirring condition, initiator is added dropwise
Aqueous solution after completion of dropwise addition, is continuously heating to 60-70 DEG C, reacts 1-3h, after reaction, then phase inversion is added in cooling discharging
Agent, which stirs evenly, to get product.
3. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Organic solvent described in step (1) is toluene or dimethylbenzene；Silane coupling agent is 3- mercapto propyl trimethoxy silicon
Alkane or 3- mercaptopropyltriethoxysilanes, silane coupling agent are 2 with attapulgite mass ratio:1-5:1.
4. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Unsaturated acid monomer described in step (2) is acrylic acid, methacrylic acid, itaconic acid, maleic acid, rich horse
Acid, one kind in maleic anhydride or arbitrary combination.
5. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Emulsifier described in step (2) is sorbitan fatty acid ester or polyoxyethylene sorbitan aliphatic acid
Ester, the dosage of emulsifier account for the 2-8% of unsaturated acid monomer mass.
6. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Crosslinking agent described in step (2) is diallyl phthalate, and crosslinking agent quality accounts for unsaturated acid monomer
The 0.1%-0.25% of quality.
7. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Organic solvent described in step (2) is 120# gasoline, 200# gasoline, one kind in kerosene, 5# white oils, insatiable hunger
With acid monomer and organic solvent mass ratio 0.25:1-0.6:1.
8. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Initiator described in step (2) is Cericammoniumsulfate or ammonium ceric nitrate, and initiator quality accounts for unsaturated acid monomer
The 0.5%-1.0% of quality.
9. a kind of cerium salt as claimed in claim 2 causes the preparation method of attapulgite/polyacrylic complex thickener,
It is characterized in that：Phase inversion agent described in step (2) is isomerous tridecanol polyoxyethylene ether or fatty alcohol polyoxyethylene ether, dosage
Account for the 4-6% of unsaturated acid monomer mass.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116835A (en) * | 2019-12-10 | 2020-05-08 | 常州大学 | Preparation method of photo-initiated attapulgite/polyacrylic acid composite thickener |
| CN112827367A (en) * | 2021-01-22 | 2021-05-25 | 武汉钜能科技有限责任公司 | Diatomite modified polyvinyl chloride composite separation membrane with high thermal stability and preparation method thereof |
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|---|---|---|---|---|
| CN102443120A (en) * | 2011-08-15 | 2012-05-09 | 中北大学 | Method for realizing efficient graft polymerization of acrylonitrile on surface of silica gel microparticles by utilizing mercapto-Ce(IV) salt redox initiation system |
| CN105061662A (en) * | 2015-08-11 | 2015-11-18 | 常州大学 | Preparation method of acrylic thickening agents with inorganic clay as cross-linking agent |
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2018
- 2018-02-06 CN CN201810118693.2A patent/CN108409899B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443120A (en) * | 2011-08-15 | 2012-05-09 | 中北大学 | Method for realizing efficient graft polymerization of acrylonitrile on surface of silica gel microparticles by utilizing mercapto-Ce(IV) salt redox initiation system |
| CN105061662A (en) * | 2015-08-11 | 2015-11-18 | 常州大学 | Preparation method of acrylic thickening agents with inorganic clay as cross-linking agent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116835A (en) * | 2019-12-10 | 2020-05-08 | 常州大学 | Preparation method of photo-initiated attapulgite/polyacrylic acid composite thickener |
| CN111116835B (en) * | 2019-12-10 | 2022-05-20 | 常州大学 | Preparation method of photo-initiated attapulgite/polyacrylic acid composite thickening agent |
| CN112827367A (en) * | 2021-01-22 | 2021-05-25 | 武汉钜能科技有限责任公司 | Diatomite modified polyvinyl chloride composite separation membrane with high thermal stability and preparation method thereof |
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