CN102504078A - Method for preparing electrolyte-resisting thickening agent - Google Patents
Method for preparing electrolyte-resisting thickening agent Download PDFInfo
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- CN102504078A CN102504078A CN201110312036XA CN201110312036A CN102504078A CN 102504078 A CN102504078 A CN 102504078A CN 201110312036X A CN201110312036X A CN 201110312036XA CN 201110312036 A CN201110312036 A CN 201110312036A CN 102504078 A CN102504078 A CN 102504078A
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- 238000000034 method Methods 0.000 title abstract description 11
- 239000002562 thickening agent Substances 0.000 title abstract description 8
- 230000008719 thickening Effects 0.000 claims abstract description 66
- 239000000463 material Substances 0.000 claims abstract description 54
- 239000000178 monomer Substances 0.000 claims abstract description 41
- 239000003792 electrolyte Substances 0.000 claims abstract description 34
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 33
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 27
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims abstract description 11
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007762 w/o emulsion Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 32
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 27
- 238000011109 contamination Methods 0.000 claims description 24
- 239000004160 Ammonium persulphate Substances 0.000 claims description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 14
- PFRGXCVKLLPLIP-UHFFFAOYSA-N diallyl disulfide Chemical compound C=CCSSCC=C PFRGXCVKLLPLIP-UHFFFAOYSA-N 0.000 claims description 14
- 235000010265 sodium sulphite Nutrition 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 13
- 235000011187 glycerol Nutrition 0.000 claims description 12
- 238000006386 neutralization reaction Methods 0.000 claims description 12
- 238000009775 high-speed stirring Methods 0.000 claims description 10
- 239000003350 kerosene Substances 0.000 claims description 10
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 7
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 5
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- -1 dodecyl allyl sulphonic acid Chemical compound 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical group OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- NWGKJDSIEKMTRX-MDZDMXLPSA-N Sorbitan oleate Chemical group CCCCCCCC\C=C\CCCCCCCC(=O)OCC(O)C1OCC(O)C1O NWGKJDSIEKMTRX-MDZDMXLPSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000007639 printing Methods 0.000 abstract description 10
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 abstract 1
- 238000012688 inverse emulsion polymerization Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000002585 base Substances 0.000 description 11
- 239000002002 slurry Substances 0.000 description 11
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 8
- 238000009835 boiling Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000011056 performance test Methods 0.000 description 8
- 125000000129 anionic group Chemical group 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 238000007720 emulsion polymerization reaction Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 235000010413 sodium alginate Nutrition 0.000 description 2
- 239000000661 sodium alginate Substances 0.000 description 2
- 229940005550 sodium alginate Drugs 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002522 swelling effect Effects 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- TUXJTJITXCHUEL-UHFFFAOYSA-N disperse red 11 Chemical compound C1=CC=C2C(=O)C3=C(N)C(OC)=CC(N)=C3C(=O)C2=C1 TUXJTJITXCHUEL-UHFFFAOYSA-N 0.000 description 1
- 238000012674 dispersion polymerization Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000012673 precipitation polymerization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a method for preparing an electrolyte-resisting thickening agent according to an inverse emulsion polymerization method. The method comprises the following steps: adding acrylamide monomer, N,N-methylene bisacrylamide, allyl sulfoacid functional monomer, oil-phase solvent, glycerol and emulsifier into a neutralized acrylic monomer aqueous solution; quickly stirring till uniformly mixing the materials, thereby forming water-in-oil emulsion; adding an initiator and triggering a polymerization reaction; adding an emulsifying dispersing agent; and cooling, thereby obtaining the thickening agent. The printing thickening agent provided by the invention has the advantages of excellent thickening capability, electrolyte-resisting capability, water-maintaining property, low viscosity drop under high electrolyte content and less dosage.
Description
Technical field
The present invention relates to technical field of textile printing, particularly a kind of preparation method who is used for the thickening material of textile printing.
Background technology
In the textile printing, for being delivered to pigment, pharmaceutical chemicals and auxiliary agent etc. on the fabric, obtain decorative pattern profile clearly, printing paste will have certain Consistency, and this just need add thickening material when the allotment mill base.Thickening material except thickening capabilities, the electrolyte-resistant ability of having relatively high expectations, to reduce consumption, reduce cost, to reduce outside the influence of printing the thing feel, also requires the system of its thickening to have the higher water-based of embracing in printing technology.Embrace after water-based is meant that slurry after the thickening material thickening is printed on the fabric ability that does not spread, keeps original decorative pattern contour sharpness towards periphery because of the capillary effect and the surperficial electrolytical effect of fabric.
What printing thickening agent used at first is native starch and sodium-alginate, but because native starch slurrying difficulty, sodium-alginate price height and facile hydrolysis, the synthetic thickening material more and more comes into one's own.Synthetic thickening agent is divided into anionic and non-ionic type synthetic thickening agent; Compound method has letex polymerization, reversed emulsion polymerization, precipitation polymerization method, liquid dispersion polymerization etc.; Develop best with the effect of anionic polyacrylic acid monomers salt thickening material so far, wherein best with the thickening effectiveness of the product of reversed emulsion polymerization gained.Contain a large amount of carboxyls on the main chain of anionic polyacrylic acid monomers salt thickening material, by the charge repulsion that these carboxyls produce under ionized state, molecular chain fully stretches; Hydrodynamic volume increases; Swelling action takes place, and the system viscosity rises, and thickening effectiveness is obvious.The stamp field is widely used at present is the anionic synthetic thickening agent; But employed synthetic thickening material need consume a large amount of energy in process of production; Produce a large amount of environmentally hazardous TX10s (APEO) simultaneously, be unfavorable for energy-conservation and environment protection.And because synthetic thickening material product electrolyte-resistant not, viscosity is not high, and usage quantity is bigger, and use cost is higher, the textiles color and luster of printing partially secretly and feel poor.Thereby to develop cheap, thickening material that consumption is few, use properties is good be the focus of present textile printing and dyeing industry.
Patent CN1624237A utilizes reversed emulsion polymerization to prepare Acrylic Acid Monomer class thickening material, though its electrolyte-resistant performance increases, its armful water effect and thickening effectiveness are limited; Patent CN101538807A utilizes reversed emulsion polymerization to prepare anionic Acrylic Acid Monomer class thickening material; Owing in polymer segment, introduce tertiary amine group and vinyl group; Improved armful outlet capacity and the electrolyte-resistant ability of thickening material, but thickening effectiveness is not good enough; Patent CN101613433A, CN101698980A, CN101736608A, CN101775099A and CN101886345A utilize the reversed-phase emulsion copolymerization method to prepare anionic Acrylic Acid Monomer class thickening material; Introduce polyether segment and adopt little crosslinking technological at its molecule segment; Make its electrolyte-resistant and an armful water-based that raising arranged; But the monomer component of its preparation raw material is complicated, and condition is wayward, and thickening effectiveness is still not good enough.And according to its mechanism of action, this type of thickening material is if use under electrolyte environment, and then its thickening effectiveness is not obvious, and the electrolyte-resistant effect is undesirable.
Summary of the invention
It is relatively poor so that the unconspicuous technical deficiency of its thickening effectiveness in particular surroundings provides a kind of new thickening material compound method to the objective of the invention is to overcome this type of thickening material electrolyte-resistant.
Technical scheme of the present invention is: in aqueous sodium hydroxide solution and in the Acrylic Acid Monomer aqueous solution of crossing, add acrylamide monomer; Add linking agent, allyl sulphonic acid function monomer, oil phase solvent, glycerine, emulsifying agent high-speed stirring subsequently it is mixed, form water-in-oil emulsion; Add initiator solution again, after polyreaction, add emulsifying dispersant, cooling makes the potential resistance to electrolyte contamination thickening material.
The degree of neutralization of the Acrylic Acid Monomer aqueous solution of wherein said neutralization is 70%-85%; The mass percentage concentration of aqueous sodium hydroxide solution is 20%-30%; The N-process temperature is not higher than 50 ℃, and the mass ratio of acrylamide monomer and Acrylic Acid Monomer is 20%-30% ~ 70%-80%.
Wherein said allyl sulphonic acid function monomer be diallyl disulfide for sulfonic acid or dodecyl allyl sulphonic acid, its consumption accounts for the 5%-20% of Acrylic Acid Monomer and acrylamide monomer total mass.
Wherein said dosage of crosslinking agent accounts for the 0.1%-0.5% of Acrylic Acid Monomer and acrylamide monomer total mass; The oil phase solvent load accounts for the 20%-25% of Acrylic Acid Monomer and acrylamide monomer total mass; The glycerine consumption accounts for the 5%-10% of Acrylic Acid Monomer and acrylamide monomer total mass, and the emulsifying agent consumption accounts for the 4%-8% of Acrylic Acid Monomer and acrylamide monomer total mass.
Described linking agent is a N,N methylene bis acrylamide, and the oil phase solvent is a kerosene, and emulsifying agent is a sorbester p17.
The mass concentration of wherein said initiator solution is 1%～10%; Described initiator solution is the mixing solutions of ammonium persulphate and sodium sulfite anhy 96; Wherein the mass ratio of ammonium persulphate and sodium sulfite anhy 96 is 4:1 ~ 9:1, and the total mass of ammonium persulphate and sodium sulfite anhy 96 accounts for 0.5%～1% of Acrylic Acid Monomer and acrylamide monomer total mass.
Wherein said emulsifying dispersant is isomerous tridecanol polyoxyethylene ether, isomery ten polyoxyethylenated alcohol or AEO, and the consumption of emulsifying dispersant accounts for the 4%-8% of Acrylic Acid Monomer and acrylamide monomer total mass.
Wherein said polymerization reaction time is 3h-6h, and temperature is 50 ℃-70 ℃, is cooled to 40 ℃ behind the adding emulsifying dispersant.
Adopt method of the present invention to prepare the potential resistance to electrolyte contamination thickening material, Acrylic Acid Monomer-acrylamide monomer copolyreaction causes easily, reacts more complete; Add the little amount of crosslinking agent N,N methylene bis acrylamide, make polymkeric substance that little crosslinking structure take place; Further increase molecular structure, in polymer molecular chain, introduce the allyl sulphonic acid function monomer, neutralize through alkali; Make its ionize have a large amount of charge generation charge repulsions, molecular chain fully stretches, and hydrodynamic volume increases; Swelling action takes place, and the system viscosity rises, and thickening effectiveness is obvious.Sulfonic introducing simultaneously, the electrolyte-resistant performance of increase system.Therefore the potential resistance to electrolyte contamination thickening material thickening effectiveness that makes is obvious, and the potential resistance to electrolyte contamination ability is strong, does contrast, excellent product performance with commercially available synthetic type of thickening material.Its performance perameter contrasts as follows:
| ? | 5% white slurry viscosity | 5% mill base viscosity |
| Commercially available certain thickening material | 35000mPa.s | 1500mPa.s |
| Thickening material of the present invention | ＞120000mPa.s | ＞8000mPa.s |
5% white slurry viscosity: 10g thickening material+190g water
5% mill base viscosity: 10g thickening material+190g water+8g Disperse Red S-5BL
Embodiment:
Below in conjunction with embodiment content of the present invention is further described.
Embodiment 1:
In the 500ml four-hole boiling flask, add the 75g Acrylic Acid Monomer, slowly add mass concentration and be 20% aqueous sodium hydroxide solution 146g, controlled temperature is no more than 50 ℃, and degree of neutralization is 70%, adds acrylamide monomer 25g; Add N,N methylene bis acrylamide 0.14g, diallyl disulfide subsequently for sulfonic acid 10g, kerosene 20g, glycerine 5g, emulsifier span 80 4g, high-speed stirring forms water-in-oil emulsion under 500 rev/mins of rotating speeds; Add the mass concentration that is made into by ammonium persulphate 0.45g, sodium sulfite anhy 96 0.05g again and be 5% initiator solution; Drip off in 1 hour; 65 ℃ of temperature of reaction were added dropwise to complete post-polymerization 4 hours, added emulsifying dispersant AEO 4g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 126000mPa.s, 5% mill base viscosity 8100mPa.s.
Embodiment 2:
In the 500ml four-hole boiling flask, add the 70g Acrylic Acid Monomer, slowly adding mass concentration is 25% aqueous sodium hydroxide solution 109g, and controlled temperature is no more than 50 ℃, and degree of neutralization is 70%, adds acrylamide monomer 30g; Add N,N methylene bis acrylamide 0.5g subsequently,, dodecyl allyl sulphonic acid 15g, kerosene 25g, glycerine 8g, emulsifier span 80 6g, high-speed stirring forms water-in-oil emulsion under 800 rev/mins of rotating speeds; 1% initiator solution that adds the mass concentration that is made into by ammonium persulphate 0.83g, sodium sulfite anhy 96 0.17g again and be; Drip off in 1 hour; 70 ℃ of temperature of reaction were added dropwise to complete post-polymerization 3 hours, added emulsifying dispersant AEO 4g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 128000mPa.s, 5% mill base viscosity 8300mPa.s.
Embodiment 3:
In the 500ml four-hole boiling flask, add the 75g Acrylic Acid Monomer, slowly adding mass concentration is 30% aqueous sodium hydroxide solution 104g, and controlled temperature is no more than 50 ℃, and degree of neutralization is 75%, adds acrylamide monomer 25g; Add N,N methylene bis acrylamide 0.1g, diallyl disulfide subsequently for sulfonic acid 5g, kerosene 20g, glycerine 10g, emulsifier span 80 8g, high-speed stirring forms water-in-oil emulsion under 1000 rev/mins of rotating speeds; Add the mass concentration that is made into by ammonium persulphate 0.5g, sodium sulfite anhy 96 0.1g again and be 3% initiator solution; Drip off in 1 hour; 70 ℃ of temperature of reaction were added dropwise to complete post-polymerization 3.5 hours, added isomerous tridecanol polyoxyethylene ether 6g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 122000mPa.s, 5% mill base viscosity 8100mPa.s.
Embodiment 4:
In the 500ml four-hole boiling flask, add the 80g Acrylic Acid Monomer, slowly adding mass concentration is 20% aqueous sodium hydroxide solution 167g, and degree of neutralization is 75%, and controlled temperature is no more than 50 ℃, adds acrylamide monomer 20g; Add N,N methylene bis acrylamide 0.2g, dodecyl allyl sulphonic acid 20g, kerosene 22g, glycerine 5g, emulsifier span 80 6g subsequently, high-speed stirring forms water-in-oil emulsion under 1500 rev/mins of rotating speeds; Add the mass concentration that is made into by ammonium persulphate 0.62g, sodium sulfite anhy 96 0.1g again and be 10% initiator solution; Drip off in 1 hour; 60 ℃ of temperature of reaction were added dropwise to complete post-polymerization 4 hours, added isomerous tridecanol polyoxyethylene ether 8g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 130000mPa.s, 5% mill base viscosity 9000mPa.s.
Embodiment 5:
In the 500ml four-hole boiling flask, add the 75g Acrylic Acid Monomer, slowly adding mass concentration is 25% aqueous sodium hydroxide solution 125g, and degree of neutralization is 75%, and controlled temperature is no more than 50 ℃, adds acrylamide monomer 25g; Add N subsequently; N-methylene-bisacrylamide 0.3g, diallyl disulfide are for sulfonic acid 15g, kerosene 25g, glycerine 5g, emulsifier span 80 4g, and high-speed stirring forms water-in-oil emulsion under 1000 rev/mins of rotating speeds, and adding the mass concentration that is made into by ammonium persulphate 0.75g, sodium sulfite anhy 96 0.15g is 4% aqueous solution; Drip off in 1 hour; 65 ℃ of temperature of reaction were added dropwise to complete post-polymerization 4 hours, added isomery ten polyoxyethylenated alcohol 6g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 132000mPa.s, 5% mill base viscosity 8900mPa.s.
Embodiment 6:
In the 500ml four-hole boiling flask, add the 80g Acrylic Acid Monomer, slowly adding mass concentration is 20% aqueous sodium hydroxide solution 178g, and degree of neutralization is 80%, and controlled temperature is no more than 50 ℃, adds acrylamide monomer 20g; Add N,N methylene bis acrylamide 0.2g, dodecyl allyl sulphonic acid 10g, kerosene 22g, glycerine 8g, emulsifier span 80 6g subsequently, high-speed stirring forms water-in-oil emulsion under 2000 rev/mins of rotating speeds; Add the mass concentration that is made into by ammonium persulphate 0.44g, sodium sulfite anhy 96 0.06g again and be 3% initiator solution; Drip off in 1 hour; 50 ℃ of temperature of reaction were added dropwise to complete post-polymerization 6 hours, added isomery ten polyoxyethylenated alcohol 4g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 128000mPa.s, 5% mill base viscosity 8600mPa.s.
Embodiment 7:
In the 500ml four-hole boiling flask, add the 70g Acrylic Acid Monomer, slowly adding mass concentration is 30% aqueous sodium hydroxide solution 110g, and degree of neutralization is that 85% controlled temperature is no more than 50 ℃, adds acrylamide monomer 30g; Add N,N methylene bis acrylamide 0.3g, diallyl disulfide subsequently for sulfonic acid 20g, kerosene 20g, glycerine 10g, emulsifier span 80 8g, high-speed stirring forms water-in-oil emulsion under 900 rev/mins of rotating speeds; Add the mass concentration that is made into by ammonium persulphate 0.48g, sodium sulfite anhy 96 0. 12g again and be 5% initiator solution; Drip off in 1 hour; 70 ℃ of temperature of reaction were added dropwise to complete post-polymerization 5 hours, added isomery ten polyoxyethylenated alcohol 8g; Naturally be cooled to 40 ℃, make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 125000mPa.s, 5% mill base viscosity 8250mPa.s.
Embodiment 8:
In the 500ml four-hole boiling flask, add the 76g Acrylic Acid Monomer, slowly adding mass concentration is 20% aqueous sodium hydroxide solution 180g, and degree of neutralization is 85%, and controlled temperature is no more than 50 ℃, adds acrylamide monomer 24g; Add N,N methylene bis acrylamide 0.1g, diallyl disulfide subsequently for sulfonic acid 8g, kerosene 25g, glycerine 8g, emulsifier span 80 4g, high-speed stirring forms water-in-oil emulsion under 1200 rev/mins of rotating speeds; Add the mass concentration that is made into by ammonium persulphate 0.75g, sodium sulfite anhy 96 0.15g again and be 5% initiator solution; Drip off in 1 hour; 60 ℃ of temperature of reaction; Be added dropwise to complete post-polymerization 6 hours, and added isomerous tridecanol polyoxyethylene ether 6g, be cooled to 40 ℃ naturally and make the potential resistance to electrolyte contamination thickening material.
Thickening material performance test: 5% white slurry viscosity 132000mPa.s, 5% mill base viscosity 9200mPa.s.
Claims (10)
1. the preparation method of a potential resistance to electrolyte contamination thickening material may further comprise the steps:
In aqueous sodium hydroxide solution and in the Acrylic Acid Monomer aqueous solution of crossing, add acrylamide monomer; Add linking agent, allyl sulphonic acid function monomer, oil phase solvent, glycerine, emulsifying agent high-speed stirring subsequently it is mixed, form water-in-oil emulsion; Add initiator solution again, after polyreaction, add emulsifying dispersant, cooling makes the potential resistance to electrolyte contamination thickening material.
2. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1 is characterized in that: the degree of neutralization of the Acrylic Acid Monomer aqueous solution of said neutralization is 70%-85%, and the mass percentage concentration of aqueous sodium hydroxide solution is 20%-30%.
3. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1 is characterized in that: the mass ratio of said acrylamide monomer and Acrylic Acid Monomer is 20%-30% ~ 70%-80%.
4. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1; It is characterized in that: said allyl sulphonic acid function monomer be diallyl disulfide for sulfonic acid or dodecyl allyl sulphonic acid, its consumption accounts for the 5%-20% of Acrylic Acid Monomer and acrylamide monomer total mass.
5. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1; It is characterized in that: dosage of crosslinking agent accounts for the 0.1%-0.5% of Acrylic Acid Monomer and acrylamide monomer total mass; The oil phase solvent load accounts for the 20%-25% of Acrylic Acid Monomer and acrylamide monomer total mass; The glycerine consumption accounts for the 5%-10% of Acrylic Acid Monomer and acrylamide monomer total mass, and the emulsifying agent consumption accounts for the 4%-8% of Acrylic Acid Monomer and acrylamide monomer total mass.
6. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1 is characterized in that: described linking agent is a N,N methylene bis acrylamide, and the oil phase solvent is a kerosene, and emulsifying agent is a sorbester p17.
7. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1 is characterized in that: the mass concentration of said initiator solution is 1%～10%.
8. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1; It is characterized in that: described initiator solution is the mixing solutions of ammonium persulphate and sodium sulfite anhy 96; Wherein the mass ratio of ammonium persulphate and sodium sulfite anhy 96 is 4:1 ~ 9:1, and the total mass of ammonium persulphate and sodium sulfite anhy 96 accounts for 0.5%～1% of Acrylic Acid Monomer and acrylamide monomer total mass.
9. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1; It is characterized in that: said emulsifying dispersant is isomerous tridecanol polyoxyethylene ether, isomery ten polyoxyethylenated alcohol or AEO, and its consumption accounts for the 4%-8% of Acrylic Acid Monomer and acrylamide monomer total mass.
10. the preparation method of potential resistance to electrolyte contamination thickening material according to claim 1 is characterized in that: described polymerization reaction time is 3h-6h, and temperature is 50 ℃-70 ℃, is cooled to 40 ℃ behind the adding emulsifying dispersant.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110312036 CN102504078B (en) | 2011-10-16 | 2011-10-16 | Method for preparing electrolyte-resisting thickening agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110312036 CN102504078B (en) | 2011-10-16 | 2011-10-16 | Method for preparing electrolyte-resisting thickening agent |
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| Publication Number | Publication Date |
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| CN102504078A true CN102504078A (en) | 2012-06-20 |
| CN102504078B CN102504078B (en) | 2013-12-18 |
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| CN 201110312036 Active CN102504078B (en) | 2011-10-16 | 2011-10-16 | Method for preparing electrolyte-resisting thickening agent |
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| CN104695249A (en) * | 2015-03-06 | 2015-06-10 | 徐饶春 | Printing thickening agent |
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| CN105073788B (en) * | 2013-02-21 | 2017-07-28 | S.P.C.M.股份公司 | The method of the weak low concentration inverse emulsion polymerization for neutralizing polymer and the reversed-phase emulsion obtained |
| CN107236074A (en) * | 2017-06-22 | 2017-10-10 | 安徽银力铸造有限公司 | A kind of preparation method of high temperature resistant potential resistance to electrolyte contamination five-membered copolymer thickener |
| CN110590226A (en) * | 2019-10-17 | 2019-12-20 | 霍邱县方博新型建材有限公司 | Preparation method of cement mortar additive for novel block wall |
| CN112642355A (en) * | 2020-12-14 | 2021-04-13 | 唐苏英 | Preparation method of cosmetic emulsifying thickener |
| CN114000367A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN115198543A (en) * | 2022-07-18 | 2022-10-18 | 苏州联胜化学有限公司 | High-performance pigment printing synthetic thickener and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105073788B (en) * | 2013-02-21 | 2017-07-28 | S.P.C.M.股份公司 | The method of the weak low concentration inverse emulsion polymerization for neutralizing polymer and the reversed-phase emulsion obtained |
| CN104695249A (en) * | 2015-03-06 | 2015-06-10 | 徐饶春 | Printing thickening agent |
| CN106279523A (en) * | 2015-06-25 | 2017-01-04 | 中国石油天然气股份有限公司 | A kind of thickening agent and its preparation method and application |
| CN106279523B (en) * | 2015-06-25 | 2019-03-15 | 中国石油天然气股份有限公司 | A kind of thickener and its preparation method and application |
| CN107236074A (en) * | 2017-06-22 | 2017-10-10 | 安徽银力铸造有限公司 | A kind of preparation method of high temperature resistant potential resistance to electrolyte contamination five-membered copolymer thickener |
| CN110590226A (en) * | 2019-10-17 | 2019-12-20 | 霍邱县方博新型建材有限公司 | Preparation method of cement mortar additive for novel block wall |
| CN112642355A (en) * | 2020-12-14 | 2021-04-13 | 唐苏英 | Preparation method of cosmetic emulsifying thickener |
| CN114000367A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN114000367B (en) * | 2021-11-09 | 2023-08-04 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN115198543A (en) * | 2022-07-18 | 2022-10-18 | 苏州联胜化学有限公司 | High-performance pigment printing synthetic thickener and preparation method thereof |
| CN115198543B (en) * | 2022-07-18 | 2023-09-12 | 苏州联胜化学有限公司 | High-performance pigment printing synthetic thickener and preparation method thereof |
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