CN105061662B - A kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent - Google Patents
A kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent Download PDFInfo
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- CN105061662B CN105061662B CN201510489209.3A CN201510489209A CN105061662B CN 105061662 B CN105061662 B CN 105061662B CN 201510489209 A CN201510489209 A CN 201510489209A CN 105061662 B CN105061662 B CN 105061662B
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Abstract
The invention belongs to field of new is and in particular to a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent.The method is modified to inorganic clay using silane coupler, introduce vinyl on its surface, then with vinyl silicane coupling agent modified inorganic clay as cross-linking agent, acrylic monomer is main monomer, hydrophobicity long-chained monomer is the function monomer improving thickening agent electrolyte resistance, prepares acrylic thickener using inverse emulsion polymerization.Gained thickening agent not only low price, and thickening properties, salt resistant character are excellent.
Description
Technical field
The invention belongs to field of new is and in particular to a kind of acrylic thickener with inorganic clay as cross-linking agent
Preparation method.
Background technology
Acrylic thickener is the class efficient thickeners developing rapidly in recent years, has thickening effect good, comprehensive
Close the feature of excellent performance, be widely used in fields such as textile printing and dyeing, leather finish, building coatings.In thickening agent building-up process,
Cross-linking agent would generally be added.Conventional cross-linking agent has：Diallyl phthalate, N, N '-di-2-ethylhexylphosphine oxide propionic acid amide..Cross-linking agent
Addition can be remarkably reinforced the anti-shear ability of thickening agent, but have document to point out that the addition of cross-linking agent can frequently result in thickening effect
Reduction.Additionally, the electrolyte-resistant ability of acrylic thickener, electrolyte resistance is being required with some higher necks
Domain, such as textile reactive printing, its application is restricted.
Content of the invention
The present invention is directed to the deficiencies in the prior art, there is provided a kind of acrylic thickener with inorganic clay as cross-linking agent
Preparation method, with inorganic clay as cross-linking agent, inorganic clay has good thixotropy and plasticity to the method, can with organic
Macromolecule thickener synergism reaches mutual supplement with each other's advantages, can reduce production cost simultaneously；In the preparation process of thickening agent, add
Hydrophobicity long-chained monomer, improves the electrolyte resistance of product using the space structure of hydrophobicity long chain alkyl group.
The technical scheme realizing above-mentioned purpose is：A kind of preparation of the acrylic thickener with inorganic clay as cross-linking agent
Method, is modified to inorganic clay initially with silane coupler, introduces vinyl on its surface, then gathers in reversed-phase emulsion
During closing preparation acrylic thickener, modified inorganic clay is added.
A kind of preparation method of acrylic thickener with inorganic clay as cross-linking agent that the present invention provides, including following
Step：
(1) add 2mol/L NaCl solution in round-bottomed flask, add inorganic clay, inorganic clay is molten with sodium chloride
The mass volume ratio of liquid is calculated as 1 with g/mL:40-1:80, stir 6-8h, discard the supernatant, washing precipitation, 50-80 DEG C of vacuum
It is dried to obtain sodio clay, sample is ground, cross 200 mesh sieves, standby；
Wherein, inorganic clay is one of bentonite, attapulgite, Kaolin；
(2) by sodio clay with solid-liquid mass ratio 1:10-1:30 are scattered in organic solvent, ultrasonic disperse 10-30min,
Deca silane coupler, using glacial acetic acid regulation system pH value to 4.0-5.0,70-100 DEG C of reaction 6-10h；After reaction terminates,
Remove solvent, vacuum drying, grind, cross 200 mesh sieves, obtain final product silane coupler modified inorganic clay；
Wherein, organic solvent is toluene or dimethylbenzene；Silane coupler is selected from VTES, vinyl three
Methoxy silane, vinyl three ('beta '-methoxy ethyoxyl) silane, silane coupler and sodio clay mass ratio are 2:1-5:
1；
(3) four-hole boiling flask is placed in psychrolusia, adds unsaturated acid monomer, hydrophobicity long-chained monomer, silane coupled
Agent modified inorganic clay, silane coupler modified inorganic clay consumption accounts for the 5%-20% of unsaturated acidity monomer mass, slowly
Deca ammonia is to solution ph 6-7；Add oil phase solvent, emulsifying agent span80, the consumption of emulsifying agent accounts for unsaturated acid monomer
The 4-6% of quality, 1000-1500 rev/min of high speed emulsifying 60-90min；It is warming up to 50-60 DEG C, in 300-450 rev/min of stirring bar
Under part, Deca initiator solution, after completion of dropwise addition, it is continuously heating to 60-70 DEG C, react 1-3h, after reaction terminates, cool down out
Material, is subsequently adding phase inversion agent and stirs and get product；
Wherein, unsaturated acid monomer is acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, maleic anhydride
One of or combination in any；
Wherein, hydrophobicity long-chained monomer is (methyl) acrylic acid C8-C16 positive structure even carbon alcohol ester, and its general structure is：
In formula, R is H or-CH3, n is the even number of 7-15；The consumption of hydrophobicity long-chained monomer accounts for unsaturated acid monomer matter
The 1%-5% of amount；Oil phase solvent is 120# gasoline, 200# gasoline, one of kerosene, 5# white oil, and oil phase solvent load accounts for not
The 60%-80% of saturation acidity monomer mass；The mass concentration of initiator solution is 5%-10%, and described initiator is water-soluble
Liquid is the mixed solution of Ammonium persulfate. or sodium peroxydisulfate and sodium sulfite, wherein, Ammonium persulfate. or sodium peroxydisulfate and sulfurous acid
The mass ratio of hydrogen sodium is:4:1-8:1, initiator gross mass accounts for the 0.5%-1.0% of unsaturated acidity monomer mass；Phase inversion agent is
One of TX-10, tween80, tween60, isomerous tridecanol polyoxyethylene ether, fatty alcohol-polyoxyethylene ether, its consumption accounts for
The 4-6% of unsaturated acidity monomer mass.
The invention has the beneficial effects as follows：
(1) adopt vinyl silicane coupling agent modified inorganic clay as cross-linking agent, not only reduce the cost of thickening agent,
And the excellent thixotropy of inorganic clay can improve the thickening effect of acrylic thickener.
(2) in the building-up process of thickening agent, improve the resistance to of acrylic thickener by adding hydrophobicity long-chained monomer
Electrolyte ability.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.It should be understood that these embodiments are intended merely to
Illustrate the present invention, rather than limit the scope of the present invention by any way.
Embodiment 1
(1) add 2mol/L NaCl solution in round-bottomed flask, add bentonite, bentonite and sodium chloride solution
Mass volume ratio is calculated as 1 with g/mL:40, stir 6h, discard the supernatant, washing precipitation, it is swollen that 50 DEG C of vacuum drying obtain sodio
Profit soil, sample is ground, and crosses 200 mesh sieves, standby.
(2) by sodium bentonite with solid-liquid mass ratio 1:10 are scattered in toluene, ultrasonic disperse 10min, Deca vinyl
Triethoxysilane, silane coupler and sodium bentonite mass ratio are 2:1, using glacial acetic acid regulation system pH value to 4.0,
70 DEG C of reaction 10h.After reaction terminates, remove solvent, vacuum drying, grind, cross 200 mesh sieves, obtain final product silane coupler modified swollen
Profit soil.
(3) four-hole boiling flask is placed in psychrolusia, adds acrylic acid, Process Conditions of Cetane Acrylate, silane coupler modified swelling
Soil, Process Conditions of Cetane Acrylate and silane coupler modified bentonite account for the 1% and 5% of acrylic monomerss quality respectively, are slowly added dropwise
Ammonia is to solution ph 6；120# gasoline, span80,120# gasoline and span80 is added to account for acrylic monomerss quality respectively
60% and 4%, 1000 revs/min of high speed emulsifying 90min, are warming up to 50 DEG C, under 300 revs/min of stirring conditions, Deca mass concentration
5% initiator solution, the redox system that initiator is made up of sodium peroxydisulfate and sodium sulfite, both mass ratios
For 4:1, initiator gross mass accounts for the 0.5% of acrylic monomerss quality, after completion of dropwise addition, is continuously heating to 60 DEG C, reacts 3h, instead
After should terminating, cooling discharging, it is subsequently adding to account for acrylic acid quality 4% phase inversion agent TX-10 and stir and get product.
Comparative example 1
Four-hole boiling flask is placed in psychrolusia, adds acrylic acid, Process Conditions of Cetane Acrylate, N, N '-di-2-ethylhexylphosphine oxide propionic acid amide., third
Olefin(e) acid hexadecyl ester and N, N '-di-2-ethylhexylphosphine oxide propionic acid amide. accounts for the 1% and 5% of acrylic monomerss quality respectively, is slowly added dropwise ammonia extremely
Solution ph 6；120# gasoline, span80,120# gasoline and span80 is added to account for 60% He of acrylic monomerss quality respectively
4%；1000 revs/min of high speed emulsifying 90min；It is warming up to 50 DEG C, under 300 revs/min of stirring conditions, Deca mass concentration 5%
Initiator solution, the redox system that initiator is made up of sodium peroxydisulfate and sodium sulfite, both mass ratios are 4:
1, initiator gross mass accounts for the 0.5% of acrylic monomerss quality, after completion of dropwise addition, is continuously heating to 60 DEG C, reacts 3h, reaction knot
Shu Hou, cooling discharging, it is subsequently adding to account for acrylic acid quality 4% phase inversion agent TX-10 and stir and get product.
Comparative example 2a
During inverse emulsion polymerization, without Process Conditions of Cetane Acrylate, other processes are identical with comparative example 1.
Comparative example 2b
In step (3), without Process Conditions of Cetane Acrylate, remaining step is all same as Example 1.
Embodiment 2
(1) add 2mol/L NaCl solution in round-bottomed flask, add attapulgite, attapulgite is molten with sodium chloride
The mass volume ratio of liquid is calculated as 1 with g/mL:80, stir 8h, discard the supernatant, washing precipitation, 80 DEG C of vacuum drying obtain sodium
Based attapulgite, sample is ground, and crosses 200 mesh sieves, standby.
(2) by sodio attapulgite with solid-liquid mass ratio 1:30 are scattered in dimethylbenzene, ultrasonic disperse 30min, Deca second
Thiazolinyl trimethoxy silane, silane coupler and sodio attapulgite mass ratio are 5:1, using glacial acetic acid regulation system pH value
To 5.0,100 DEG C of reaction 6h.After reaction terminates, remove solvent, vacuum drying, grind, cross 200 mesh sieves, obtain final product silane coupler
Attapulgite modified.
(3) four-hole boiling flask is placed in psychrolusia, adds methacrylic acid, tetradecyl methylacrylate, silane coupler
Attapulgite modified, tetradecyl methylacrylate and attapulgite modified by silane coupling agent account for methacrylic acid quality respectively
5% and 20%, it is slowly added dropwise ammonia to solution ph 7；Add 200# gasoline, emulsifying agent span80,200# gasoline and span80
Account for the 80% and 6% of methacrylic acid quality respectively, 1500 revs/min of high speed emulsifying 60min；It is warming up to 60 DEG C, at 450 revs/min
Under stirring condition, the initiator solution of Deca mass concentration 10%, initiator is made up of Ammonium persulfate. and sodium sulfite
Redox system, both mass ratios are 8:1, initiator gross mass accounts for the 1.0% of acrylic monomerss quality, completion of dropwise addition
Afterwards, it is continuously heating to 70 DEG C, react 1h, after reaction terminates, cooling discharging, it is subsequently adding and account for methacrylic acid quality 6% phase inversion
Agent tween80 stirs and gets product.
Embodiment 3
(1) add 2mol/L NaCl solution in round-bottomed flask, add Kaolin, Kaolin and sodium chloride solution
Mass volume ratio is calculated as 1 with g/mL:60, stir 7h, discard the supernatant, washing precipitation, 70 DEG C of vacuum drying obtain sodio height
Ridge soil, sample is ground, and crosses 200 mesh sieves, standby.
(2) by sodio Kaolin with solid-liquid mass ratio 1:20 are scattered in toluene, ultrasonic disperse 20min, Deca vinyl
Three ('beta '-methoxy ethyoxyl) silane, silane coupler and sodio Kaolin mass ratio are 4:1, body is adjusted using glacial acetic acid
It is that pH value reacts 8h to 4.5,80 DEG C.After reaction terminates, remove solvent, vacuum drying, grind, cross 200 mesh sieves, obtain final product silane even
Connection agent modified kaolin.
(3) four-hole boiling flask is placed in psychrolusia, adds itaconic acid, dodecyl acrylate, silane coupler modified kaolinite
Soil, dodecyl acrylate and silane coupler modified Kaolin account for the 2% and 10% of itaconic acid monomer mass respectively, are slowly added dropwise
Ammonia is to solution ph 6.5；Kerosene, span80, kerosene and span80 is added to account for 70% He of itaconic acid monomer mass respectively
5%, 1200 revs/min of high speed emulsifying 80min；It is warming up to 55 DEG C, under 350 revs/min of stirring conditions, Deca mass concentration 8%
Initiator solution, the redox system that initiator is made up of Ammonium persulfate. and sodium sulfite, both mass ratios are 6:
1, initiator gross mass accounts for the 0.6% of acrylic monomerss quality, after completion of dropwise addition, is continuously heating to 65 DEG C, reacts 2h, reaction knot
Shu Hou, cooling discharging, it is subsequently adding to account for itaconic acid quality 5% phase inversion agent tween60 and stir and get product.
Embodiment 4
(1) add 2mol/L NaCl solution in round-bottomed flask, add bentonite, bentonite and sodium chloride solution
Mass volume ratio is calculated as 1 with g/mL:70, stir 6.5h, discard the supernatant, washing precipitation, 60 DEG C of vacuum drying obtain sodio
Bentonite, sample is ground, and crosses 200 mesh sieves, standby.
(2) by sodium bentonite with solid-liquid mass ratio 1:25 are scattered in dimethylbenzene, ultrasonic disperse 15min, Deca ethylene
Ethyl triethoxy silicane alkane, silane coupler and sodium bentonite mass ratio are 3:1, using glacial acetic acid regulation system pH value extremely
4.0,90 DEG C of reaction 7h.After reaction terminates, remove solvent, vacuum drying, grind, cross 200 mesh sieves, obtain final product silane coupler modified
Bentonite.
(3) four-hole boiling flask is placed in psychrolusia, adds maleic acid, 1-Octyl acrylate, silane coupler modified bentonite,
1-Octyl acrylate and silane coupler modified bentonite consumption account for the 3% and 15% of maleic acid monomer quality respectively, are slowly added dropwise
Ammonia is to solution ph 6；5# white oil, span80,5# white oil and span80 consumption is added to account for maleic acid monomer quality respectively
65% and 4.5%, 1300 revs/min of high speed emulsifying 70min；It is warming up to 58 DEG C, under 400 revs/min of stirring conditions, Deca quality is dense
Degree 6% initiator solution, the redox system that initiator is made up of sodium peroxydisulfate and sodium sulfite, both quality it
Than for 5:1, initiator gross mass accounts for the 0.8% of maleic acid monomer quality, after completion of dropwise addition, is continuously heating to 70 DEG C, reaction
1.5h, after reaction terminates, cooling discharging, it is subsequently adding account for maleic acid monomer quality 4.5% phase inversion agent AEO3 and stir
Get product.
Embodiment 5
Accurately weigh 2g thickening agent, add 98g distilled water, stirring Deca 3-4 drips ammonia, it is sufficiently stirred for being made into quality and divide
The white slurry of number 2%.With Brookfield DV- II+Pro viscometer, in 10 revs/min of constant rotational speed (No. 6 rotors), survey under room temperature
The viscosity of ding white ware slurry.
Electrolyte resistance is represented with viscosity retention ratio, measures above-mentioned thickening agent and starches addition 0.05%NaCl (solid) in vain in vain
Slurry viscosity, viscosity retention ratio=ηPlus after NaCl/ηPlus before NaCl, viscosity retention ratio is higher, and electrolyte-resistant is better.
Table 1 sample thickening properties
As can be seen from the above table, embodiment 1-4 gained thickening agent has very strong thickening capabilities, and electrolyte resistance is excellent
Different.Because inorganic clay has certain thickening properties in itself, therefore, the thickening properties of embodiment 1-4 gained thickening agent are excellent
In the comparative example 1, the comparative example 2a that are not added with inorganic clay cross-linking agent.In comparative example 1, with the addition of hydrophobicity long-chained monomer, thickening
The thickening capabilities of agent, electrolyte resistance are preferable；And in comparative example 2a, it is not added with hydrophobicity long-chained monomer, the resistance to electricity of thickening agent
Solution matter poor performance；Although being not added with hydrophobicity long-chained monomer in comparative example 2b, but due to the presence of inorganic clay cross-linking agent,
Gained thickening agent still has preferable electrolyte resistance.
Claims (9)
1. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent it is characterised in that：Methods described
Concretely comprise the following steps,
(1) add 2mol/L NaCl solution in round-bottomed flask, add inorganic clay, inorganic clay and sodium chloride solution
Mass volume ratio is calculated as 1 with g/mL:40-1:80, stir 6-8h, discard the supernatant, washing precipitation, 50-80 DEG C of vacuum drying
Obtain sodio clay, sample is ground, cross 200 mesh sieves, standby；
(2) by sodio clay with solid-liquid mass ratio 1:10-1:30 are scattered in organic solvent, ultrasonic disperse 10-30min, Deca
Silane coupler, using glacial acetic acid regulation system pH value to 4.0-5.0,70-100 DEG C of reaction 6-10h；After reaction terminates, remove
Solvent, vacuum drying, grind, cross 200 mesh sieves, obtain final product silane coupler modified inorganic clay；
(3) four-hole boiling flask is placed in psychrolusia, adds unsaturated acid monomer, hydrophobicity long-chained monomer, silane coupler to change
Property inorganic clay, silane coupler modified inorganic clay consumption accounts for the 5%-20% of unsaturated acidity monomer mass, is slowly added dropwise
Ammonia is to solution ph 6-7；Add oil phase solvent, emulsifying agent span80, the consumption of emulsifying agent accounts for unsaturated acidity monomer mass
4-6%, 1000-1500 rev/min of high speed emulsifying 60-90min；It is warming up to 50-60 DEG C, in 300-450 rev/min of stirring condition
Under, Deca initiator solution, after completion of dropwise addition, it is continuously heating to 60-70 DEG C, react 1-3h, after reaction terminates, cool down out
Material, is subsequently adding phase inversion agent and stirs and get product.
2. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Inorganic clay described in step (1) is one of bentonite, attapulgite, Kaolin.
3. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Organic solvent described in step (2) is toluene or dimethylbenzene.
4. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Silane coupler described in step (2) is selected from VTES, vinyltrimethoxy silane, second
Thiazolinyl three ('beta '-methoxy ethyoxyl) silane, silane coupler and sodio clay mass ratio are 2:1-5:1.
5. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Unsaturated acid monomer described in step (3) be acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid,
One of maleic anhydride or combination in any.
6. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Hydrophobicity long-chained monomer described in step (3) is (methyl) acrylic acid C8-C16 positive structure even carbon alcohol ester, its knot
Structure formula is：
In formula, R is H or-CH3, n is the even number of 7-15；The consumption of hydrophobicity long-chained monomer accounts for unsaturated acidity monomer mass
1%-5%.
7. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Oil phase solvent described in step (3) is 120# gasoline, 200# gasoline, one of kerosene, 5# white oil, and oil phase is molten
Agent consumption accounts for the 60%-80% of unsaturated acidity monomer mass.
8. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：The mass concentration of the initiator solution described in step (3) is 5%-10%, and described initiator solution was
Ammonium sulfate or the mixed solution of sodium peroxydisulfate and sodium sulfite, wherein, Ammonium persulfate. or sodium peroxydisulfate and sodium sulfite
Mass ratio is 4:1-8:1, initiator gross mass accounts for the 0.5%-1.0% of unsaturated acidity monomer mass.
9. a kind of preparation method of the acrylic thickener with inorganic clay as cross-linking agent as claimed in claim 1, it is special
Levy and be：Phase inversion agent described in step (3) is TX-10, tween80, tween60, in isomerous tridecanol polyoxyethylene ether
One kind, its consumption accounts for the 4-6% of unsaturated acidity monomer mass.
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Effective date of registration: 20211222 Address after: Room 407-2-6, building C, Tian'an Digital City, 588 Changwu South Road, Wujin high tech Industrial Development Zone, Changzhou City, Jiangsu Province 213100 Patentee after: CHANGZHOU XIAOGUO INFORMATION SERVICES Co.,Ltd. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: CHANGZHOU University |