CN101935357A - Preparation method of high tackifying cationic guar gum - Google Patents
Preparation method of high tackifying cationic guar gum Download PDFInfo
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- CN101935357A CN101935357A CN 201010276330 CN201010276330A CN101935357A CN 101935357 A CN101935357 A CN 101935357A CN 201010276330 CN201010276330 CN 201010276330 CN 201010276330 A CN201010276330 A CN 201010276330A CN 101935357 A CN101935357 A CN 101935357A
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Abstract
The invention relates to a preparation method of high tackifying cationic guar gum, which is characterized by comprising the following compositions in parts by weight: 2-12 parts of guar gum, 10-80 parts of activator which adopts a water solution of inorganic base with the mass concentration of 0.1-3 percent, 10-50 parts of organic solvent, 0.5-12 parts of cationic reagent and 0.5-10 parts of hydrophobic cationic reagent. Hydrophobic modified cationic guar gum is prepared through macromolecule chemical reaction by adopting the hydrophobic reagent and the cationic reagent and utilizing active hydroxyl on a guar gum molecule. By introducing long-chain hydrophobic alkyl in the guar gum molecule, a physical crosslinked network is formed by utilizing the chain entanglement association reaction between every two molecules, and therefore, the invention fulfills better tackifying function on the guar gum, reduces positive ionization to lower the influence of molecular weight to the product performance, greatly enhances the tackifying performance of the cationic guar gum and has better application prospect as an environmental-friendly coating thickener, a shampoo conditioner, a shampoo thickener, a retention aid in papermaking, a wastewater treatment fluocculant and the like.
Description
One. technical field
The present invention relates to a kind of preparation method of water-soluble polymers, belong to the Polymer Synthesizing field.
Two. background technology
Guar gum is a kind of natural galactomannan gum that obtains that extracts from the endosperm that originates in ground guar seeds such as India, Pakistan, its molecule is by being main chain backbone with (1-4)-β-D-seminose, single α-D-semi-lactosi is a side chain, and links to each other with main chain and constitute with (1-6) key.Guar gum is dispersed in the water, form high viscosity liquid, the viscosity of 1% solution reaches 5～6Pas, is that the natural gum medium viscosity of discovery at present is the highest, is widely used in oil production, food-processing, daily-use chemical industry, papermaking, weaving and medicine and other fields as thickening material, stablizer, emulsifying agent.
Cation guar gum is a class important function natural macromolecular material, U.S. Pat 4198253 has been introduced the preparation method of cation guar gum, and it is used for shampoo, Liquid soap, body wash as amendment, and in papermaking, cook retention aid, in oil production, make oil-displacing agent three times.The Zhao Yan of Shaanxi Tech Univ Na, the Jiangsu chemical industry, 2007 (35), prepared the cation-modified guar gum of good water solubility with phase transfer catalysis process.The Ma Bingjie of college of science of Shenyang University of Technology etc., Harbin Institute of Technology's journal, 2009 (41), with the guar gum is raw material, and 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is an etherifying agent, and sodium hydroxide is catalyzer, ethanol is solvent, has prepared the quaternary ammonium salt cationic guar gum, has investigated its preparation condition.Ten thousand Xiao Fangs of South China Science ﹠ Engineering University etc., fine chemistry industry, 2006 (23), synthesizing new retention filtration adjuvant-cationic hydroxyethyl guar gum, the viscosity of positively charged ion etherificate product and the influence factor of nitrogen massfraction have been studied, determined cationization reaction optimal conditions, the cation guar gum viscosity of gained 1wt% can reach 3700mpa.s.Find that in the cation guar gum preparation with in using the positive ionization process under alkaline condition reduces the guar gum molecular weight, thereby influences its thickening property and result of use.By in the guar gum molecule, introducing the hydrophobic alkyl and the quaternary ammonium cation group of long-chain, utilize its intermolecular chain entanglement to form physical cross-linked network, can play certain thickening power to guar gum solution, reduce cationization and make the influence of molecular weight reduction product property.Therefore, by molecular designing and synthesising process research, adopt methods of hydrophobilization, the JR-125 that obtains high tackify is a key of the present invention.
Three. summary of the invention
The objective of the invention is to provide a kind of preparation method of high tackify JR-125 at the deficiencies in the prior art, be characterized in adopting hydrophobization reagent and cationic reagent, utilize the activity hydroxy on the guar gum molecule to pass through the high tackify JR-125 of macromolecular chemistry prepared in reaction, effectively improve the tackifying of JR-125.
The object of the invention is realized that by following technical measures wherein said raw material mark is parts by weight except that specified otherwise.
The initial synthesis material recipe ingredient of high tackify JR-125 is:
Guar gum 2-12 part
It is aqueous solution 10-80 part of the mineral alkali of 0.1-3% that activator adopts mass concentration
Organic solvent 10-50 part
Cationic reagent 0.5-12 part
Dewatering cationic reagent 0.5-10 part
Wherein, guar gum can adopt common guar gum, hydroxyethyl guar gum, any in the Rhoximat RH 148.
Activator is a sodium hydroxide, any in potassium hydroxide or the sodium bicarbonate.
Organic solvent can adopt in ethanol, Virahol, propyl carbinol, butanone, the dimethyl sulfoxide (DMSO) any.
Cationic reagent can adopt the epoxypropyl tri alkyl ammomium chloride, and its alkyl carbon atom quantity is 1-5.
Dewatering cationic reagent can adopt epoxypropyl tri alkyl ammomium chloride or the functionalized cationic nitrogen compound of chloro-hydrin(e), its alkyl R
1And R
2Carbon atom quantity is 1-5, R
3Carbon atom quantity is 6-24.
High tackify JR-125 preparation method:
Guar gum (GG) 2-12 part and the adding of organic solvent 10-50 part are had in the three-necked bottle of agitator and thermometer mechanical stirring 0.5-2 hour.Under agitation slowly adding concentration is 0.1-3% activator aqueous solution 10-80 part, logical nitrogen is warming up to 40-80 ℃, treats the GG swelling 0.5-2 hour, dewatering cationic reagent 0.5-10 part or cationic reagent 0.5-12 part/dewatering cationic reagent 0.5-10 part, reacted 1-7 hour, inclining product, is neutralized to PH=7-8 with hydrochloric acid, filter, the employing organic solvent washing soaks, and removes Residual reactants, in vacuum drying oven in 30-60 ℃ of dry 3-7 hour.
The performance of high tackify JR-125:
Adopting epoxypropyl dimethyl cetyl chloride ammonium (DA16), is that matrix carries out the dewatering cationic graft modification with hydroxypropylguar gum (HGG), and research has prepared the guar gum with higher apparent viscosity.As shown in Figure 1, there is a tangible critical association concentration (Cp*:0.6wt%) in the dewatering cationic Rhoximat RH 148,, increases with polymer concentration below the concentration at this, and it is slow that its apparent viscosity increases trend; When polymer concentration reaches Cp* when above, apparent viscosity rises rapidly, shows tangible tackify effect.The apparent viscosity of the HGG-g-DA16 solution of 1wt% is up to 12057mpa.s, the viscosity of purer HGG about 4000mpa.s that rises.
The present invention has following advantage:
The present invention adopts hydrophobization reagent and cationic reagent, utilizes the activity hydroxy on the guar gum molecule to pass through macromolecular chemistry prepared in reaction dewatered modified cation guar gum.By in the guar gum molecule, introducing the hydrophobic alkyl of long-chain, utilize its intermolecular chain entanglement association to form physical cross-linked network, guar gum is played viscosifying action preferably, reduce cationization and make the influence of molecular weight reduction product property, significantly improve the thickening property of JR-125, have application promise in clinical practice as environmental protection coating material thickening material, shampoo-conditioner and thickening material, Retention Aid in Papermaking, sewage treatment flocculating agent etc.
Four. description of drawings
Fig. 1 modified cation guar gum apparent viscosity and polymer concentration relation
Five. embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the content of the invention described above.
Guar gum (GG) 30 grams and dehydrated alcohol 100 gram addings are had in the three-necked bottle of agitator and thermometer mechanical stirring 0.5 hour.Under agitation slowly add concentration and be 1% the NaOH aqueous solution 800 grams, logical nitrogen, be warming up to 60 ℃, treated the GG swelling 1.5 hours, slowly add the epoxypropyl dimethyl dodecyl chlorination ammonium of 100 grams, reacted 0.5 hour, slowly add 30 gram epoxypropyl triethyl ammonium chlorides again, continue reaction 4 hours, inclining product, be neutralized to PH=7 with glacialacetic acid, filter.Adopt dehydrated alcohol, washing with acetone to soak, remove Residual reactants, in vacuum drying oven in 60 ℃ of dryings 3 hours.
Embodiment 2
Guar gum (GG) 120 grams and dimethyl sulfoxide (DMSO) 200 gram addings are had in the three-necked bottle of agitator and thermometer mechanical stirring 1.5 hours.Under agitation slowly add concentration and be 3% the KOH aqueous solution 500 grams, logical nitrogen is warming up to 80 ℃, treated the GG swelling 0.5 hour, and slowly added 3-chloro-2-hydroxypropyl-octyl alkyl dimethyl ammonium chloride 40 grams, reacted 7 hours, inclining product, is neutralized to PH=7 with hydrochloric acid, filters.Adopt normal hexane, washing with acetone to soak, remove Residual reactants, in vacuum drying oven in 30 ℃ of dryings 5 hours.
Embodiment 3
80 kilograms of guar gums (GG) and butanone 500 gram addings are had in the three-necked bottle of agitator and thermometer mechanical stirring 2 hours.Under agitation slowly add concentration and be 1% the NaOH aqueous solution 300 grams, logical nitrogen, be warming up to 50 ℃, treated the GG swelling 2 hours, slowly add the epoxypropyl dimethylhexane ammonium chloride of 10 grams, reacted 3 hours, slowly add 50 gram epoxypropyl trimethylammonium chloride ammoniums again, reacted 1 hour, inclining product, be neutralized to PH=7-8 with hydrochloric acid, filter.Adopt normal hexane, propyl carbinol washing to soak, remove Residual reactants, in vacuum drying oven in 50 ℃ of dryings 7 hours.
Embodiment 4
Guar gum (GG) 60 grams and Virahol 300 gram addings are had in the three-necked bottle of agitator and thermometer logical nitrogen, mechanical stirring 1 hour.Under agitation slowly add concentration and be 0.2% sodium bicarbonate aqueous solution 100 grams, be warming up to 40 ℃, treated the GG swelling 1 hour, slowly add 3-chloro-2-hydroxypropyl-eicosyl diethyl ammonium chloride 70 grams, reacted 5 hours, inclining product, be neutralized to PH=7-8 with dilute sulphuric acid acid, filter.Adopt normal hexane, absolute ethanol washing to soak, remove Residual reactants, in vacuum drying oven in 70 ℃ of dryings 4 hours.
Claims (7)
1. high tackify JR-125 is characterized in that the raw material of synthetic this high tackify JR-125 is composed of the following components, is by weight:
Guar gum 2-12 part
It is aqueous solution 10-80 part of the mineral alkali of 0.1-3% that activator adopts mass concentration
Organic solvent 10-50 part
Cationic reagent 0.5-12 part
Dewatering cationic reagent 0.5-10 part
2. high according to claim 1 tackify JR-125 is characterized in that the synthetic used guar gum of this high tackify JR-125 is common guar gum, hydroxyethyl guar gum, any in the Rhoximat RH 148.
3. high according to claim 1 tackify JR-125 is characterized in that the synthetic used activator of this high tackify JR-125 is a sodium hydroxide, any in potassium hydroxide or the sodium bicarbonate.
4. high according to claim 1 tackify JR-125, it is characterized in that the synthetic used organic solvent of this high tackify JR-125 be in dehydrated alcohol, Virahol, propyl carbinol, butanone, the dimethyl sulfoxide (DMSO) any.
5. high according to claim 1 tackify JR-125 is characterized in that used cationic reagent is arranged is the epoxypropyl tri alkyl ammomium chloride to synthetic this high tackify JR-125, and its alkyl carbon atom quantity is 1-5.
6. high tackify JR-125 as described in requiring 1 as patent is characterized in that the synthetic used dewatering cationic reagent of this high tackify JR-125 is the functionalized cationic nitrogen compound of epoxypropyl tri alkyl ammomium chloride or chloro-hydrin(e), its alkyl R
1And R
2Carbon atom quantity is 1-5, R
3Carbon atom quantity is 6-24.
7. as the preparation method of high tackify JR-125 as described in the claim 1～6, it is characterized in that this method may further comprise the steps:
Guar gum (GG) 2-12 part and the adding of organic solvent 10-50 part are had in the three-necked bottle of agitator and thermometer, mechanical stirring 0.5-2 hour, under agitation slowly adding concentration is 0.1-3% activator aqueous solution 10-80 part, logical nitrogen, be warming up to 40-80 ℃, treated the GG swelling 0.5-2 hour, dewatering cationic reagent 0.5-10 part or cationic reagent 0.5-12 part/dewatering cationic reagent 0.5-10 part, reacted 1-7 hour, inclining product, is neutralized to PH=7-8 with hydrochloric acid, filter, the employing organic solvent washing soaks, and removes Residual reactants, in vacuum drying oven in 30-60 ℃ of dry 3-7 hour.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172251A (en) * | 2013-04-23 | 2013-06-26 | 四川大学 | Novel chitosan-based sludge dewatering flocculant and preparation method thereof |
| CN103524634A (en) * | 2013-09-28 | 2014-01-22 | 昆山市周市溴化锂溶液厂 | Preparation method for guar gum for fabric caring |
| CN103788220A (en) * | 2012-11-05 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of instant hydroxypropyl guar |
| CN104130337A (en) * | 2014-07-25 | 2014-11-05 | 山东广浦生物科技有限公司 | Method for preparing carboxymethyl hydroxypropyl guar gum powder by guar gum sheet one-step method |
| CN109517082A (en) * | 2017-09-18 | 2019-03-26 | 中国石油化工股份有限公司 | A kind of non-long linear alkyl hydrophobically modified hydroxyethyl guar gum thickener and preparation method thereof |
| CN110408059A (en) * | 2019-08-05 | 2019-11-05 | 海洋石油工程股份有限公司 | Submarine pipeline isolation blocks pigging material and preparation method thereof |
| CN111448220A (en) * | 2017-12-06 | 2020-07-24 | 花王株式会社 | Polysaccharide derivatives |
| US11359166B2 (en) | 2017-12-06 | 2022-06-14 | Kao Corporation | Fabric treatment composition |
| US11655435B2 (en) | 2017-12-06 | 2023-05-23 | Kao Corporation | Hydroxy alkyl cellulose soil release agent with a cationic group and a C4—C12 hydrophobic group |
| US11655434B2 (en) | 2017-12-06 | 2023-05-23 | Kao Corporation | Composition |
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| US5387675A (en) * | 1993-03-10 | 1995-02-07 | Rhone-Poulenc Specialty Chemicals Co. | Modified hydrophobic cationic thickening compositions |
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2010
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Patent Citations (1)
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|---|---|---|---|---|
| US5387675A (en) * | 1993-03-10 | 1995-02-07 | Rhone-Poulenc Specialty Chemicals Co. | Modified hydrophobic cationic thickening compositions |
Non-Patent Citations (1)
| Title |
|---|
| 《上海应用技术学院学报》 20060630 姚天平等 阳离子瓜耳胶的合成 第93页第2.2.2部分 1-7 第6卷, 第2期 2 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788220A (en) * | 2012-11-05 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of instant hydroxypropyl guar |
| CN103788220B (en) * | 2012-11-05 | 2016-12-21 | 中国石油化工股份有限公司 | A kind of preparation method of Instant hydroxypropyl guar gum |
| CN103172251A (en) * | 2013-04-23 | 2013-06-26 | 四川大学 | Novel chitosan-based sludge dewatering flocculant and preparation method thereof |
| CN103524634A (en) * | 2013-09-28 | 2014-01-22 | 昆山市周市溴化锂溶液厂 | Preparation method for guar gum for fabric caring |
| CN104130337A (en) * | 2014-07-25 | 2014-11-05 | 山东广浦生物科技有限公司 | Method for preparing carboxymethyl hydroxypropyl guar gum powder by guar gum sheet one-step method |
| CN109517082B (en) * | 2017-09-18 | 2021-04-13 | 中国石油化工股份有限公司 | Non-long linear chain alkyl hydrophobically modified hydroxyethyl guar gum thickener and preparation method thereof |
| CN109517082A (en) * | 2017-09-18 | 2019-03-26 | 中国石油化工股份有限公司 | A kind of non-long linear alkyl hydrophobically modified hydroxyethyl guar gum thickener and preparation method thereof |
| US11359166B2 (en) | 2017-12-06 | 2022-06-14 | Kao Corporation | Fabric treatment composition |
| CN111448220A (en) * | 2017-12-06 | 2020-07-24 | 花王株式会社 | Polysaccharide derivatives |
| US11401350B2 (en) | 2017-12-06 | 2022-08-02 | Kao Corporation | Polysaccharide derivative |
| US11655435B2 (en) | 2017-12-06 | 2023-05-23 | Kao Corporation | Hydroxy alkyl cellulose soil release agent with a cationic group and a C4—C12 hydrophobic group |
| US11655434B2 (en) | 2017-12-06 | 2023-05-23 | Kao Corporation | Composition |
| CN110408059A (en) * | 2019-08-05 | 2019-11-05 | 海洋石油工程股份有限公司 | Submarine pipeline isolation blocks pigging material and preparation method thereof |
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