CN104928951A - Preparation method for organic-inorganic composite printing thickener - Google Patents
Preparation method for organic-inorganic composite printing thickener Download PDFInfo
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Abstract
The invention relates to a preparation method for organic-inorganic composite printing thickener. The method comprises the steps that firstly, purification and surface carboxylation are performed on inorganic thickener powder which is low in cost; secondly, in the process of polymerization preparation of polyacrylic thickener by means of inverse emulsion, surface-carboxylation inorganic thickener is added to prepare the organic-inorganic composite printing thickener. According to the organic-inorganic composite printing thickener obtained by the preparation method, not only is the cost low, but also the thickening performance and salt-resistance performance are excellent.
Description
Technical field
The present invention relates to a kind of textile printing field, be specifically related to a kind of preparation method of Organic-inorganic composite printing thickening agent.
Background technology
In printing in textiles process, in order to obtain pattern clearly, in print paste except the chemical agent of necessity, also to add suitable thickener to increase the viscosity of print paste, reducing its mobility, prevent the imbibition of dyestuff.The performance of printing thickening agent directly affects the COLOR FASTNESS, feel, tinctorial yield etc. of Printing.The printing thickening agent used the earliest is mainly native starch and sodium alginate, due to native starch slurrying difficulty, after stamp terminates, and the off difference of thickener; And sodium alginate price is high, the too high degraded easily causing strand of paste producing temperature.Therefore, in stamp industry, urgent need selectivity is excellent, cheap thickener substitutes.
Inorganic thickening agent is a class imbibition and forms thixotropic gel mineral, these mineral generally have the trellis of layer structure or expansion, when disperseing in water, metal ion is wherein from platelet to external diffusion, along with the carrying out of aquation occurs swelling, to being finally separated completely with platelet, form soliquid.Because of its low price, have a wide range of applications in water paint field.Because inorganic thickening agent thickening properties cannot meet technology for printing fabric requirement, limit its application in printing in textiles industry.
Polyacrylic synthetic thickening agent has into the features such as paste ability is strong, easily washing performance is good, PRINTED FABRIC feel is good, be widely used, but its fancy price adds stamp cost in printing in textiles field.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, cheap inorganic thickening agent is added in the preparation process of polyacrylic synthetic thickening agent, the Organic-inorganic composite printing thickening agent that preparation cost performance is high.
The preparation method of a kind of Organic-inorganic composite printing thickening agent provided by the invention, comprises the following steps:
(1) inorganic thickening agent powder is joined in the sodium hexametaphosphate solution of mass concentration 50-80g/L, the mass ratio of inorganic thickening agent powder and water is 1:50-1:100, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 100-250W ultrasonic power, sonic oscillation 1-2h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, with distilled water washing 3-5 time, dry at 80-100 DEG C, ground 200 mesh sieves, obtain purifying inorganic thickening agent powder;
Above-mentioned inorganic thickening agent powder is the one in bentonite, attapulgite, kaolin;
(2) 2g purifying inorganic thickening agent powder and 50-100mL organic solvent are placed in 250mL round-bottomed flask, ultrasonic process 30-60min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, be made into the dimercaptosuccinic acid solution of mass concentration 1-2g/L, then dimercaptosuccinic acid solution is added drop-wise in above-mentioned inorganic thickening agent suspension, drips after terminating, at 25-40 DEG C, stir 12-24h, after reaction terminates, add ethyl acetate in the solution, centrifugation, precipitation is with after distilled water washing 3-5 time, again be dispersed in 10-20mL deionized water, obtain the inorganic thickening agent suspension of surface carboxyl groups;
Above-mentioned organic solvent is toluene or dimethylbenzene;
Above-mentioned dimercaptosuccinic acid is 1:1-3:1 with the ratio of inorganic thickening agent powder quality;
(3) in the inorganic thickening agent suspension of above-mentioned surface carboxyl groups, add unsaturated acid monomer, by ammoniacal liquor adjust ph to 6-7, high-speed stirred 1-2h, obtains aqueous-phase material; Emulsifying agent, crosslinking agent and organic solvent are made into oil phase, under stirring condition, aqueous-phase material is added in oil phase, after 1000-1500 rev/min of emulsify at a high speed 60-90min, drip initiator solution, drip after terminating, under 300-450 rev/min of stirring condition, 60-70 DEG C of polymerization 1-3h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
Above-mentioned unsaturated acid monomer is one in acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, maleic anhydride or any combination, and the mass ratio of unsaturated acid monomer and inorganic thickening agent powder is 5:1-50:1.
Mentioned emulsifier is the compound emulsifying agent of span80 and tween60 composition, and span80 and tween60 mass ratio is 2:1-3:1, and the consumption of compound emulsifying agent accounts for the 3-6% of unsaturated acid monomer mass.
Above-mentioned crosslinking agent is the one in diallyl phthalate, N, N-methylene-bisacrylamide, and crosslinking agent quality accounts for the 0.05%-0.1% of unsaturated acid monomer mass.
Above-mentioned organic solvent is 120# gasoline, 200# gasoline, the one in kerosene, 5# white oil, the ratio 0.6:1-0.8:1 of organic solvent and unsaturated acid monomer mass.
Above-mentioned initator is the one in potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, and initator quality accounts for the 0.5%-1.0% of unsaturated acid monomer mass.
The invention has the beneficial effects as follows:
(1) add in the preparation process of agent for polyacrylic acid thickening by inorganic thickening agent that is purified and surface carboxyl groups, the compatibility of inorganic thickening agent powder and agent for polyacrylic acid thickening is good.
(2) select cheap inorganic thickening agent powder and organic thickening agent compound, prepare Organic-inorganic composite thickener, products obtained therefrom low price, thickening properties, salt resistant character are excellent.
Detailed description of the invention
Below in conjunction with specific embodiment, in further detail the present invention is described.Should be understood that these embodiments just in order to demonstrate the invention, but not limit the scope of the invention by any way.
Embodiment 1
(1) bentonite is joined in the sodium hexametaphosphate solution of mass concentration 50g/L, the mass ratio of bentonite and water is 1:50, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 100W ultrasonic power, sonic oscillation 2h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, 3 times are washed with distilled water, dry at 80 DEG C, ground 200 mesh sieves, obtain purifying bentonite powder;
(2) 2g purifying bentonite and 50mL toluene solution are placed in 250mL round-bottomed flask, ultrasonic process 30min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, be made into the dimercaptosuccinic acid solution of mass concentration 1g/L, be then added drop-wise in above-mentioned bentonite suspension by dimercaptosuccinic acid solution, dimercaptosuccinic acid and bentonite mass ratio are 1:1, after dropping terminates, at 25 DEG C, stir 24h, after reaction terminates, add ethyl acetate in the solution, centrifugation, after precipitation distilled water washs 3 times, be again dispersed in 10mL deionized water, obtain the bentonite suspension of surface carboxyl groups; (3) in the bentonite suspension of above-mentioned surface carboxyl groups, add acrylic monomers, acrylic monomers and bentonite mass ratio are 5:1, and by ammoniacal liquor adjust ph to 6, high-speed stirred 1h, obtains aqueous-phase material; The compound emulsifying agent, diallyl phthalate and the 120# gasoline that are formed by span80 and tween60 are made into oil phase, and wherein span80 and tween60 mass ratio is 2:1, and the consumption of compound emulsifying agent accounts for 3% of acrylic monomers quality; Diallyl phthalate accounts for 0.05% of acrylic monomers quality; 120# gasoline and acrylic monomers mass ratio are 0.6:1; Under stirring condition, aqueous-phase material is added in oil phase, after 1000 revs/min of emulsify at a high speed 90min, drip ammonium persulfate aqueous solution, the quality of ammonium persulfate accounts for 0.5% of acrylic monomers quality, drips after terminating, under 300 revs/min of stirring conditions, 70 DEG C of polymerization 1h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
Comparative example 1
(1) bentonite is joined in the sodium hexametaphosphate solution of mass concentration 50g/L, the mass ratio of bentonite and water is 1:50, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 100W ultrasonic power, sonic oscillation 2h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, 3 times are washed with distilled water, dry at 80 DEG C, ground 200 mesh sieves, obtain purifying bentonite powder;
(2) 2g purifying bentonite and 50mL toluene solution are placed in 250mL round-bottomed flask, ultrasonic process 30min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, is made into the dimercaptosuccinic acid solution of mass concentration 1g/L, then dimercaptosuccinic acid solution is added drop-wise in above-mentioned bentonite suspension, dimercaptosuccinic acid and bentonite mass ratio are 1:1, after dropping terminates, at 25 DEG C, stir 24h, after reaction terminates, add ethyl acetate in the solution, centrifugation, after precipitation distilled water washs 3 times, dries at 80 DEG C, ground 200 mesh sieves, for subsequent use.
Embodiment 2
(1) attapulgite is joined in the sodium hexametaphosphate solution of mass concentration 80g/L, the mass ratio of attapulgite and water is 1:100, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 250W ultrasonic power, sonic oscillation 1h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, 5 times are washed with distilled water, dry at 100 DEG C, ground 200 mesh sieves, obtain purifying attapulgite powder;
(2) 2g purifying attapulgite powder and 100mL xylene solution are placed in 250mL round-bottomed flask, ultrasonic process 60min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, be made into the dimercaptosuccinic acid solution of mass concentration 2g/L, then dimercaptosuccinic acid solution is added drop-wise in above-mentioned attapulgite suspension, dimercaptosuccinic acid is 3:1 with the ratio of attapulgite powder quality, after dropping terminates, 12h is stirred at 40 DEG C, after reaction terminates, add ethyl acetate in the solution, centrifugation, after precipitation distilled water washs 5 times, be again dispersed in 20mL deionized water, obtain the attapulgite suspension of surface carboxyl groups;
(3) in the attapulgite suspension of above-mentioned surface carboxyl groups, add methacrylic acid monomer, the mass ratio of methacrylic acid monomer and attapulgite powder is 50:1, and by ammoniacal liquor adjust ph to 7, high-speed stirred 2h, obtains aqueous-phase material; The compound emulsifying agent, N, N-methylene-bisacrylamide and the 200# gasoline that are formed by span80 and tween60 are made into oil phase, and wherein span80 and tween60 mass ratio is 3:1, and the consumption of compound emulsifying agent accounts for 6% of methacrylic acid monomer quality; N, N-methylene-bisacrylamide accounts for 0.1% of methacrylic acid monomer quality; 200# gasoline and methacrylic acid monomer mass ratio are 0.8:1; Under stirring condition, aqueous-phase material is added in oil phase, after 1500 revs/min of emulsify at a high speed 60min, drip persulfate aqueous solution, the quality of potassium peroxydisulfate accounts for 1% of methacrylic acid monomer quality, drips after terminating, under 450 revs/min of stirring conditions, 60 DEG C of polyase 13 h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
Comparative example 2
Added by methacrylic acid monomer in four-hole boiling flask, by ammoniacal liquor adjust ph to 7, high-speed stirred 2h, obtains aqueous-phase material; The compound emulsifying agent, N, N-methylene-bisacrylamide and the 200# gasoline that are formed by span80 and tween60 are made into oil phase, and wherein span80 and tween60 mass ratio is 3:1, and the consumption of compound emulsifying agent accounts for 6% of methacrylic acid monomer quality; N, N-methylene-bisacrylamide accounts for 0.1% of methacrylic acid monomer quality; 200# gasoline and methacrylic acid monomer mass ratio are 0.8:1; Under stirring condition, aqueous-phase material is added in oil phase, after 1500 revs/min of emulsify at a high speed 60min, drip persulfate aqueous solution, the quality of potassium peroxydisulfate accounts for 1% of methacrylic acid monomer quality, drips after terminating, under 450 revs/min of stirring conditions, 60 DEG C of polyase 13 h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
Embodiment 3
(1) kaolin powder is joined in the sodium hexametaphosphate solution of mass concentration 60g/L, the mass ratio of kaolin powder and water is 1:60, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 150W ultrasonic power, sonic oscillation 1.5h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, 4 times are washed with distilled water, dry at 90 DEG C, ground 200 mesh sieves, obtain purifying kaolin powder;
(2) 2g purifying kaolin powder and 60mL toluene solution are placed in 250mL round-bottomed flask, ultrasonic process 50min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, be made into the dimercaptosuccinic acid solution of mass concentration 1.5g/L, then dimercaptosuccinic acid solution is added drop-wise in above-mentioned Kaolin clay suspension, dimercaptosuccinic acid and kaolin powder mass ratio are 2.5:1, after dropping terminates, 18h is stirred at 30 DEG C, after reaction terminates, add ethyl acetate in the solution, centrifugation, after precipitation distilled water washs 4 times, be again dispersed in 15mL deionized water, obtain the Kaolin clay suspension of surface carboxyl groups;
(3) in the Kaolin clay suspension of above-mentioned surface carboxyl groups, add itaconic acid monomer, the mass ratio of itaconic acid monomer and kaolin powder is 30:1, and by ammoniacal liquor adjust ph to 6.5, high-speed stirred 1.5h, obtains aqueous-phase material; The compound emulsifying agent, N, N-methylene-bisacrylamide and the kerosene that are formed by span80 and tween60 are made into oil phase, and wherein span80 and tween60 mass ratio is 2.5:1, and the consumption of compound emulsifying agent accounts for 5% of itaconic acid monomer mass; N, N-methylene-bisacrylamide accounts for 0.08% of itaconic acid monomer mass; Kerosene is 0.7:1 with the ratio of itaconic acid monomer mass; Under stirring condition, aqueous-phase material is added in oil phase, after 1200 revs/min of emulsify at a high speed 80min, drip sodium persulfate aqueous solution, the quality of sodium peroxydisulfate accounts for 0.8% of itaconic acid monomer mass, drips after terminating, under 400 revs/min of stirring conditions, 65 DEG C of polymerization 2h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
Embodiment 4
(1) attapulgite powder is joined in the sodium hexametaphosphate solution of mass concentration 70g/L, the mass ratio of attapulgite powder and water is 1:70, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 200W ultrasonic power, sonic oscillation 1h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, 5 times are washed with distilled water, dry at 85 DEG C, ground 200 mesh sieves, obtain purifying attapulgite powder;
(2) 2g purifying attapulgite powder and 70mL xylene solution are placed in 250mL round-bottomed flask, ultrasonic process 40min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, be made into the dimercaptosuccinic acid solution of mass concentration 1.2g/L, then dimercaptosuccinic acid solution is added drop-wise in above-mentioned attapulgite suspension, dimercaptosuccinic acid is 1.5:1 with the ratio of attapulgite powder quality, after dropping terminates, 16h is stirred at 35 DEG C, after reaction terminates, add ethyl acetate in the solution, centrifugation, after precipitation distilled water washs 3 times, be again dispersed in 18mL deionized water, obtain the attapulgite suspension of surface carboxyl groups;
(3) in the attapulgite suspension of above-mentioned surface carboxyl groups, add maleic acid monomer, the mass ratio of maleic acid monomer and attapulgite powder is 20:1, and by ammoniacal liquor adjust ph to 6, high-speed stirred 1.2h, obtains aqueous-phase material; The compound emulsifying agent, diallyl phthalate and the 5# white oil that are formed by span80 and tween60 are made into oil phase, and wherein span80 and tween60 mass ratio is 2:1, and the consumption of compound emulsifying agent accounts for 4% of maleic acid monomer quality; Diallyl phthalate accounts for 0.06% of maleic acid monomer quality; 5# white oil and maleic acid monomer mass ratio are 0.65:1; Under stirring condition, aqueous-phase material is added in oil phase, after 1400 revs/min of emulsify at a high speed 70min, drip sodium persulfate aqueous solution, the quality of sodium peroxydisulfate accounts for 0.6% of maleic acid monomer quality, drips after terminating, under 350 revs/min of stirring conditions, 60 DEG C of polymerization 2h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
Embodiment 5
Accurately take 2g thickener, add 98g distilled water, stir and drip 3-4 and drip ammoniacal liquor, fully stir the white slurry being made into mass fraction 2%.With Brookfield DV-II+Pro viscosimeter, at constant rotational speed 10 revs/min (No. 6 rotors), under room temperature, measure the viscosity of white slurry.
Electrolyte res is tance represents with viscosity retention ratio, measures above-mentioned thickener and starches in vain and add the white slurry viscosity of 0.05%NaCl (solid), viscosity retention ratio=η
after adding NaCl/ η
before adding NaCl, viscosity retention ratio is higher, and electrolyte-resistant is better.
Table 1 sample thickening properties
As can be seen from Table 1, compared with comparative example, viscosity and the viscosity retention ratio of embodiment 1-4 gained thickener are higher, and this shows, thickening capabilities, the good salt tolerance of gained Organic-inorganic composite thickener of the present invention in pure inorganic thickening agent, Polyacrylate thickeners, and are better than commercially available thickener.
Claims (10)
1. a preparation method for Organic-inorganic composite printing thickening agent, is characterized in that: first by cheap inorganic thickening agent powder purifying, surface carboxyl groups; Then prepare in the process of agent for polyacrylic acid thickening at inverse emulsion polymerization, surface carboxyl groups inorganic thickening agent is added, obtain Organic-inorganic composite printing thickening agent.
2. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 1, is characterized in that: the concrete steps of described method are,
(1) inorganic thickening agent powder is joined in the sodium hexametaphosphate solution of mass concentration 50-80g/L, the mass ratio of inorganic thickening agent powder and water is 1:50-1:100, after stirring 10min, this suspension is placed in ultrasonic oscillator, under 100-250W ultrasonic power, sonic oscillation 1-2h, after naturally leaving standstill 30min, gets upper strata suspension centrifugation, with distilled water washing 3-5 time, dry at 80-100 DEG C, ground 200 mesh sieves, obtain purifying inorganic thickening agent powder;
(2) 2g purifying inorganic thickening agent powder and 50-100mL organic solvent are placed in 250mL round-bottomed flask, ultrasonic process 30-60min, fully homogenizes; Dimercaptosuccinic acid is dissolved in dimethyl sulphoxide solution, be made into the dimercaptosuccinic acid solution of mass concentration 1-2g/L, then dimercaptosuccinic acid solution is added drop-wise in above-mentioned inorganic thickening agent suspension, drips after terminating, at 25-40 DEG C, stir 12-24h, after reaction terminates, add ethyl acetate in the solution, centrifugation, precipitation is with after distilled water washing 3-5 time, again be dispersed in 10-20mL deionized water, obtain the inorganic thickening agent suspension of surface carboxyl groups;
(3) in the inorganic thickening agent suspension of above-mentioned surface carboxyl groups, add unsaturated acid monomer, by ammoniacal liquor adjust ph to 6-7, high-speed stirred 1-2h, obtains aqueous-phase material; Emulsifying agent, crosslinking agent and organic solvent are made into oil phase, under stirring condition, aqueous-phase material is added in oil phase, after 1000-1500 rev/min of emulsify at a high speed 60-90min, drip initiator solution, drip after terminating, under 300-450 rev/min of stirring condition, 60-70 DEG C of polymerization 1-3h, after reaction terminates, cooling discharging, then adds phase inversion agent TX-10 and stirs and get product.
3. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, is characterized in that: the inorganic thickening agent powder described in step (1) is the one in bentonite, attapulgite, kaolin.
4. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, is characterized in that: the organic solvent described in step (2) is toluene or dimethylbenzene.
5. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, is characterized in that: the dimercaptosuccinic acid described in step (2) is 1:1-3:1 with the ratio of inorganic thickening agent powder quality.
6. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, it is characterized in that: the unsaturated acid monomer described in step (3) is one in acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, maleic anhydride or any combination, and the mass ratio of unsaturated acid monomer and inorganic thickening agent powder is 5:1-50:1.
7. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, it is characterized in that: the emulsifying agent described in step (3) is the compound emulsifying agent of span80 and tween60 composition, span80 and tween60 mass ratio is 2:1-3:1, and the consumption of compound emulsifying agent accounts for the 3-6% of unsaturated acid monomer mass.
8. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, it is characterized in that: the crosslinking agent described in step (3) is diallyl phthalate, N, one in N-methylene-bisacrylamide, crosslinking agent quality accounts for the 0.05%-0.1% of unsaturated acid monomer mass.
9. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, it is characterized in that: the organic solvent described in step (3) is 120# gasoline, 200# gasoline, one in kerosene, 5# white oil, the ratio 0.6:1-0.8:1 of organic solvent and unsaturated acid monomer mass.
10. the preparation method of a kind of Organic-inorganic composite printing thickening agent according to claim 2, it is characterized in that: the initator described in step (3) is the one in potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, and initator quality accounts for the 0.5%-1.0% of unsaturated acid monomer mass.
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| CN108285507A (en) * | 2018-01-26 | 2018-07-17 | 常州大学 | A kind of preparation method of attapulgite/polyacrylic complex thickener |
| CN108505365A (en) * | 2018-05-11 | 2018-09-07 | 江苏麦阁吸附剂有限公司 | A kind of preparation method of salt tolerant printing thickening agent |
| CN109355945A (en) * | 2018-09-21 | 2019-02-19 | 佛山市森昂生物科技有限公司 | A kind of printing thickening agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108505365A (en) * | 2018-05-11 | 2018-09-07 | 江苏麦阁吸附剂有限公司 | A kind of preparation method of salt tolerant printing thickening agent |
| CN108505365B (en) * | 2018-05-11 | 2020-04-28 | 江苏麦阁吸附剂有限公司 | Preparation method of salt-resistant printing thickener |
| CN109355945A (en) * | 2018-09-21 | 2019-02-19 | 佛山市森昂生物科技有限公司 | A kind of printing thickening agent |
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