CN115612032A - A kind of synthetic method of acrylic thickener - Google Patents
A kind of synthetic method of acrylic thickener Download PDFInfo
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- CN115612032A CN115612032A CN202211359919.0A CN202211359919A CN115612032A CN 115612032 A CN115612032 A CN 115612032A CN 202211359919 A CN202211359919 A CN 202211359919A CN 115612032 A CN115612032 A CN 115612032A
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- 239000002562 thickening agent Substances 0.000 title claims abstract description 45
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000010189 synthetic method Methods 0.000 title claims description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 19
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 19
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 19
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 4
- 229920000642 polymer Polymers 0.000 claims description 33
- 230000008719 thickening Effects 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012263 liquid product Substances 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- PQJJJMRNHATNKG-UHFFFAOYSA-N ethyl bromoacetate Chemical compound CCOC(=O)CBr PQJJJMRNHATNKG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001308 synthesis method Methods 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 3
- 229920000058 polyacrylate Polymers 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 description 17
- 230000008859 change Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PMBWYDCSOSTTDK-UHFFFAOYSA-N [Br].CCOC(C)=O Chemical compound [Br].CCOC(C)=O PMBWYDCSOSTTDK-UHFFFAOYSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- JXXDQMIAHQBWSW-UHFFFAOYSA-M azanium sodium sulfurous acid sulfate Chemical compound S(=O)(=O)([O-])[O-].[NH4+].S(=O)(O)O.[Na+] JXXDQMIAHQBWSW-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 229940065472 octyl acrylate Drugs 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 239000006254 rheological additive Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
本发明公开了一种丙烯酸类增稠剂的合成方法。将摩尔比为1:1~2的脂肪醇聚氧乙烯醚丙烯酸酯和丙烯酸类单体在水中混溶后加到圆底烧瓶中，之后将引发剂过硫酸铵加到反应体系中，升高油浴温度为80‑150℃，搅拌速度控制100‑500 rpm，反应1‑5 h，静置分层，取下层液体得到丙烯酸类增稠剂。本发明通过分子结构设计，得到一种丙烯酸类高分子增稠剂，产品性能优异。
The invention discloses a method for synthesizing an acrylic thickener. Add fatty alcohol polyoxyethylene ether acrylate and acrylic acid monomers with a molar ratio of 1:1~2 to the round bottom flask after miscibility in water, and then add the initiator ammonium persulfate to the reaction system to raise The temperature of the oil bath is 80-150°C, the stirring speed is controlled at 100-500 rpm, the reaction is carried out for 1-5 hours, the layers are separated after standing, and the lower liquid is taken to obtain the acrylic thickener. The invention obtains an acrylic polymer thickener through molecular structure design, and the product performance is excellent.
Description
技术领域technical field
本发明涉及一种丙烯酸类增稠剂的合成方法，属于应用化学领域。The invention relates to a method for synthesizing an acrylic thickener, belonging to the field of applied chemistry.
背景技术Background technique
增稠剂是一种流变助剂，因为在提高物系黏度或稠度方面具有增稠明显、使用方便、用量小等特点，近年来发展迅速，成为一类新型功能高分子材料。王云普等人（王云普,温慧慧,杨超,刘汉功.水性缔合型增稠剂的合成及性能研究[J].甘肃科技,2007(05):68-69+19.）以丙烯酸、丙烯酸辛酯、甲基丙烯酸甲酯和丙烯酸丁酯为单体，以反应型乳化剂，采用乳液聚合，制得一种缔合型增稠剂；汤金伟等人（汤金伟,陈晓红,冯俏君,方伟洪,程文静.聚丙烯酸增稠剂的制备及在日化中的应用[J].化学推进剂与高分子材料,2020,18(05):55-58）以丙烯酸为原料，季戊四醇三烯丙基醚为交联剂，水为溶剂，在引发剂作用下制得聚丙烯酸增稠剂。上述增稠剂对中和剂、可溶性盐和pH值都十分敏感，所以需要开发一种新型丙烯酸类增稠剂以拓宽应用范围。Thickener is a kind of rheological additive. Because it has the characteristics of obvious thickening, convenient use and small dosage in improving the viscosity or consistency of the system, it has developed rapidly in recent years and has become a new type of functional polymer material. Wang Yunpu et al. (Wang Yunpu, Wen Huihui, Yang Chao, Liu Hangong. Synthesis and performance research of water-based associative thickener[J]. Gansu Science and Technology, 2007(05):68-69+19.) Using acrylic acid and octyl acrylate , methyl methacrylate and butyl acrylate are used as monomers, and a reactive emulsifier is used for emulsion polymerization to prepare an associative thickener; Tang Jinwei et al. (Tang Jinwei, Chen Xiaohong, Feng Qiaojun, Fang Weihong, Cheng Wen Jing. Preparation of polyacrylic acid thickener and its application in daily chemicals [J]. Chemical Propellants and Polymer Materials, 2020,18(05):55-58) Using acrylic acid as raw material, pentaerythritol triallyl ether As a crosslinking agent, water is used as a solvent, and the polyacrylic acid thickener is prepared under the action of an initiator. The above-mentioned thickeners are very sensitive to neutralizers, soluble salts, and pH, so it is necessary to develop a new type of acrylic thickener to broaden the application range.
发明内容Contents of the invention
本发明旨在提供一种丙烯酸类增稠剂的合成方法。The present invention aims to provide a synthetic method of acrylic thickener.
表面活性剂是一类重要的化合物，其中非离子型表面活性剂不易受无机盐和pH值的影响，将非离子表面活性剂与丙烯酸类单体共聚得到的丙烯酸类增稠剂可以有效规避传统丙烯酸增稠剂的缺点。Surfactants are an important class of compounds, among which nonionic surfactants are not easily affected by inorganic salts and pH values. Acrylic thickeners obtained by copolymerizing nonionic surfactants with acrylic monomers can effectively avoid traditional Disadvantages of acrylic thickeners.
本发明以脂肪醇聚氧乙烯醚丙烯酸酯(AA-AEO9)和丙烯酸类单体为原料，在引发剂的作用下，得到了一类高分子聚合物增稠剂，其反应合成路线（以丙烯酸为例）如下式所示：The present invention uses fatty alcohol polyoxyethylene ether acrylate (AA-AEO 9 ) and acrylic acid monomers as raw materials, and under the action of an initiator, a class of polymer thickener is obtained, and its reaction synthesis route (with acrylic acid as an example) as shown in the following formula:
本发明提供了一种丙烯酸类增稠剂，由以下原料：脂肪醇聚氧乙烯醚丙烯酸酯和丙烯酸类单体，以水为溶剂，在引发剂作用下共聚得到聚合物增稠剂，其中脂肪醇聚氧乙烯醚丙烯酸酯与丙烯酸类单体的摩尔比为：1:1~2，两种反应单体的总质量与水的质量比为1:1~1:5，引发剂用量占两种反应单体总量的质量分数为0.1~3 %。The invention provides an acrylic thickener, which is obtained from the following raw materials: fatty alcohol polyoxyethylene ether acrylate and acrylic monomers, using water as a solvent, and copolymerizing under the action of an initiator to obtain a polymer thickener. The molar ratio of alcohol polyoxyethylene ether acrylate to acrylic monomer is 1:1~2, the mass ratio of the total mass of the two reaction monomers to water is 1:1~1:5, and the amount of initiator accounts for two The mass fraction of the total amount of reaction monomers is 0.1-3%.
进一步地，丙烯酸类单体是丙烯酸、丙烯酸丁酯、甲基丙烯酸、甲基丙烯酸甲酯中的一种。Further, the acrylic monomer is one of acrylic acid, butyl acrylate, methacrylic acid, and methyl methacrylate.
进一步地，引发剂是溴代乙酸乙酯、过硫酸铵-亚硫酸氢钠、过硫酸铵中的一种。Further, the initiator is one of ethyl bromoacetate, ammonium persulfate-sodium bisulfite, and ammonium persulfate.
本发明制备的丙烯酸类增稠剂，具有优异的增稠性能，取2wt. %的丙烯酸类增稠剂与10wt. %十二烷基苯磺酸钠LAS水溶液复配，体系的粘度能达到1050~1200 mPa·s。The acrylic thickener prepared by the present invention has excellent thickening properties. When 2wt.% of the acrylic thickener is compounded with 10wt.% sodium dodecylbenzenesulfonate LAS aqueous solution, the viscosity of the system can reach 1050 ~1200 mPa s.
本发明提供了上述丙烯酸类增稠剂的合成方法，包括以下步骤：The invention provides the synthetic method of above-mentioned acrylic thickener, comprises the following steps:
将摩尔比为1:1~2的脂肪醇聚氧乙烯醚丙烯酸酯和丙烯酸类单体溶于去离子水后加入装有机械搅拌器、温度计的圆底烧瓶中，搅拌均匀后加入引发剂，利用恒压滴液漏斗将引发剂逐步加入反应体系中，升温反应1-5 h，体相明显分层表示反应结束；反应结束后，冷却、静置，取下层液态产物，即为丙烯酸类高分子聚合物增稠剂。Dissolve fatty alcohol polyoxyethylene ether acrylate and acrylic monomers with a molar ratio of 1:1~2 in deionized water and add them to a round-bottomed flask equipped with a mechanical stirrer and a thermometer. After stirring evenly, add the initiator. Use a constant pressure dropping funnel to gradually add the initiator into the reaction system, heat up the reaction for 1-5 hours, and the bulk phase is clearly separated to indicate that the reaction is over; Molecular polymer thickener.
上述合成方法中反应的温度为80-150 ℃。The reaction temperature in the above synthesis method is 80-150°C.
上述合成方法中反应时间优选为2-4 h。The reaction time in the above synthesis method is preferably 2-4 h.
上述合成方法中反应过程中搅拌速度为100-500 rpm。In the above synthesis method, the stirring speed is 100-500 rpm during the reaction process.
本发明的有益效果：Beneficial effects of the present invention:
本发明以脂肪醇聚氧乙烯醚丙烯酸酯为原料，通过与丙烯酸类单体共聚，得到一类新型的丙烯酸类高分子增稠剂。此类增稠剂有很多优点，一方面，与一般的聚合物增稠剂相比，延长了支链，使得该高分子聚合物在表面活性剂溶液体系中的网状结构更紧密，达到增稠的作用；另一方面，与脂肪醇聚氧乙烯醚丙烯酸酯自聚得到的增稠剂相比，该高分子聚合物中更多的支链强化了体系中网状结构的结合力，而且，多样化的亲油基团进一步提升了主表面活性剂的表面活性。The invention uses fatty alcohol polyoxyethylene ether acrylate as raw material, and obtains a novel type of acrylic polymer thickener through copolymerization with acrylic monomers. This type of thickener has many advantages. On the one hand, compared with general polymer thickeners, the branched chain is extended, which makes the network structure of the high molecular polymer in the surfactant solution system tighter and achieves thickening. On the other hand, compared with the thickener obtained from the self-polymerization of fatty alcohol polyoxyethylene ether acrylate, more branched chains in the polymer strengthen the binding force of the network structure in the system, and , the diversified lipophilic groups further enhance the surface activity of the main surfactant.
附图说明Description of drawings
图1是本发明实施例1合成丙烯酸类增稠剂的红外光谱图。Fig. 1 is the infrared spectrogram of the synthetic acrylic thickener of embodiment 1 of the present invention.
图2是本发明实施例1~6合成的丙烯酸类增稠剂在10wt. %LAS水溶液中的粘度对比图。2 is a comparison diagram of the viscosity of the acrylic thickener synthesized in Examples 1-6 of the present invention in 10wt.% LAS aqueous solution.
具体实施方式detailed description
下面通过实施例来进一步说明本发明，但不局限于以下实施例。The present invention is further illustrated by the following examples, but not limited to the following examples.
实施例1：Example 1:
将脂肪醇聚氧乙烯醚丙烯酸酯30 g、丙烯酸(AA, 3.39 g)溶于去离子水中，加入到装有机械搅拌器、温度计的三口圆底烧瓶中，保持50 ℃搅拌，将0.6 g过硫酸铵加入到反应体系中，之后升温至150 ℃继续反应1 h。反应结束后，冷却、静置，得到下层液态产物。Dissolve 30 g of fatty alcohol polyoxyethylene ether acrylate and acrylic acid (AA, 3.39 g) in deionized water, add them into a three-necked round-bottomed flask equipped with a mechanical stirrer and a thermometer, keep stirring at 50 °C, and dissolve 0.6 g over Ammonium sulfate was added to the reaction system, and then the temperature was raised to 150 °C to continue the reaction for 1 h. After the reaction was completed, it was cooled and left to stand to obtain the liquid product in the lower layer.
为了验证本发明所得到的产物为丙烯酸类聚合物增稠剂，采用红外光谱分析仪对产物的结构进行了表征，如图1。由图可见，1635.5 cm-1处的碳碳双键特征峰并未出现，证明聚合反应较为完全。In order to verify that the product obtained in the present invention is an acrylic polymer thickener, the structure of the product was characterized by an infrared spectrometer, as shown in Figure 1. It can be seen from the figure that the characteristic peak of the carbon-carbon double bond at 1635.5 cm -1 does not appear, which proves that the polymerization reaction is relatively complete.
为了验证本发明所得到的聚合物具有增稠性能，取2wt. %的聚合物增稠剂与10wt. %LAS水溶液复配，用NDJ-8S数显粘度仪测得其复配前后的粘度变化，如图2。由图可见，在25℃下，LAS水溶液的粘度基本为零。In order to verify that the polymer obtained by the present invention has thickening properties, take 2wt.% polymer thickener and 10wt.% LAS aqueous solution for compounding, and measure the viscosity change before and after its compounding with NDJ-8S digital display viscometer , as shown in Figure 2. It can be seen from the figure that at 25°C, the viscosity of the LAS aqueous solution is basically zero.
为了验证本发明所得到的聚合物的增稠效果，将脂肪醇聚氧乙烯醚丙烯酸酯自聚得到的增稠剂与本实施例所得的聚合物以相同比例加入LAS中，体系的粘度分别增加到了875 mPa·s 和1135 mPa·s，证明该聚合物不仅有增稠性能，而且比脂肪醇聚氧乙烯醚丙烯酸酯自聚得到的增稠剂效果更佳。In order to verify the thickening effect of the polymer obtained in the present invention, the thickener obtained from the self-polymerization of fatty alcohol polyoxyethylene ether acrylate and the polymer obtained in this example were added to LAS in the same proportion, and the viscosity of the system increased respectively The values of 875 mPa·s and 1135 mPa·s prove that the polymer not only has thickening performance, but also has a better effect than the thickener obtained by self-polymerization of fatty alcohol polyoxyethylene ether acrylate.
实施例2：Example 2:
将脂肪醇聚氧乙烯醚丙烯酸酯30 g、丙烯酸丁酯(AA, 6.02 g)溶于去离子水中，加入到装有机械搅拌器、温度计的三口圆底烧瓶中，保持60 ℃搅拌，将0.14 g溴代乙酸乙酯加入到反应体系中，之后升温至130 ℃继续反应2 h。反应结束后，冷却、静置，得到下层液态产物。Dissolve 30 g of fatty alcohol polyoxyethylene ether acrylate and butyl acrylate (AA, 6.02 g) in deionized water, add them into a three-necked round-bottomed flask equipped with a mechanical stirrer and a thermometer, keep stirring at 60 °C, and mix 0.14 One g of ethyl bromoacetate was added to the reaction system, and then the temperature was raised to 130 °C to continue the reaction for 2 h. After the reaction was completed, it was cooled and left to stand to obtain the liquid product in the lower layer.
为了验证本发明所得到的聚合物具有增稠性能，取2wt. %的聚合物与10wt. %LAS水溶液复配，用NDJ-8S数显粘度仪测得其复配前后的粘度变化，如图2。由图可见，在25℃下，LAS水溶液的粘度基本为零。将本实施例所得的聚合物与LAS复配以后，体系的粘度增加到了1085 mPa·s，证明该聚合物确实有增稠性能。In order to verify that the polymer obtained by the present invention has thickening properties, take 2wt.% polymer and 10wt.% LAS aqueous solution for compounding, and measure the viscosity change before and after its compounding with NDJ-8S digital display viscometer, as shown in Fig. 2. It can be seen from the figure that at 25°C, the viscosity of the LAS aqueous solution is basically zero. After compounding the polymer obtained in this example with LAS, the viscosity of the system increased to 1085 mPa·s, which proves that the polymer does have thickening properties.
实施例3：Example 3:
将脂肪醇聚氧乙烯醚丙烯酸酯30 g、丙烯酸(AA, 5.08 g)溶于去离子水中，加入到装有机械搅拌器、温度计的三口圆底烧瓶中，保持50 ℃搅拌，将1.0 g过硫酸铵-亚硫酸氢钠加入到反应体系中，之后升温至110 ℃继续反应3 h。反应结束后，冷却、静置，得到下层液态产物。Dissolve 30 g of fatty alcohol polyoxyethylene ether acrylate and acrylic acid (AA, 5.08 g) in deionized water, add them into a three-necked round-bottomed flask equipped with a mechanical stirrer and a thermometer, keep stirring at 50 °C, and dissolve 1.0 g over Ammonium sulfate-sodium bisulfite was added to the reaction system, and then the temperature was raised to 110 °C to continue the reaction for 3 h. After the reaction was completed, it was cooled and left to stand to obtain the liquid product in the lower layer.
为了验证本发明所得到的聚合物具有增稠性能，取2wt. %的聚合物与10wt. %LAS水溶液复配，用NDJ-8S数显粘度仪测得其复配前后的粘度变化，如图2。由图可见，在25℃下，LAS水溶液的粘度基本为零。将本实施例所得的聚合物与LAS复配以后，体系的粘度增加到了1150 mPa·s，证明该聚合物确实有增稠性能。In order to verify that the polymer obtained by the present invention has thickening properties, take 2wt.% polymer and 10wt.% LAS aqueous solution for compounding, and measure the viscosity change before and after its compounding with NDJ-8S digital display viscometer, as shown in Fig. 2. It can be seen from the figure that at 25°C, the viscosity of the LAS aqueous solution is basically zero. After compounding the polymer obtained in this example with LAS, the viscosity of the system increased to 1150 mPa·s, which proves that the polymer does have thickening properties.
实施例4：Example 4:
将脂肪醇聚氧乙烯醚丙烯酸酯30 g、甲基丙烯酸(AA, 6.02 g)溶于去离子水中，加入到装有机械搅拌器、温度计的三口圆底烧瓶中，保持60 ℃搅拌，将0.5 g过硫酸铵加入到反应体系中，之后升温至90 ℃继续反应4 h。反应结束后，冷却、静置，得到下层液态产物。Dissolve 30 g of fatty alcohol polyoxyethylene ether acrylate and methacrylic acid (AA, 6.02 g) in deionized water, add them into a three-necked round-bottomed flask equipped with a mechanical stirrer and a thermometer, keep stirring at 60 °C, and add 0.5 g ammonium persulfate was added to the reaction system, and then the temperature was raised to 90 °C to continue the reaction for 4 h. After the reaction was completed, it was cooled and left to stand to obtain the liquid product in the lower layer.
为了验证本发明所得到的聚合物具有增稠性能，取2wt. %的聚合物与10wt. %LAS水溶液复配，用NDJ-8S数显粘度仪测得其复配前后的粘度变化，如图2。由图可见，在25℃下，LAS水溶液的粘度基本为零。将本实施例所得的聚合物与LAS复配以后，体系的粘度增加到了1115 mPa·s，证明该聚合物确实有增稠性能。In order to verify that the polymer obtained by the present invention has thickening properties, take 2wt.% polymer and 10wt.% LAS aqueous solution for compounding, and measure the viscosity change before and after its compounding with NDJ-8S digital display viscometer, as shown in Fig. 2. It can be seen from the figure that at 25°C, the viscosity of the LAS aqueous solution is basically zero. After compounding the polymer obtained in this example with LAS, the viscosity of the system increased to 1115 mPa·s, which proves that the polymer does have thickening properties.
实施例5：Example 5:
将脂肪醇聚氧乙烯醚丙烯酸酯30 g、丙烯酸(AA, 6.77 g)溶于去离子水中，加入到装有机械搅拌器、温度计的三口圆底烧瓶中，保持40 ℃搅拌，将0.3 g溴代乙酸乙酯加入到反应体系中，之后升温至80 ℃继续反应5 h。反应结束后，冷却、静置，得到下层液态产物。Dissolve 30 g of fatty alcohol polyoxyethylene ether acrylate and acrylic acid (AA, 6.77 g) in deionized water, add them into a three-necked round-bottomed flask equipped with a mechanical stirrer and a thermometer, keep stirring at 40 °C, and dissolve 0.3 g of bromine Ethyl acetate was added to the reaction system, and then the temperature was raised to 80 °C to continue the reaction for 5 h. After the reaction was completed, it was cooled and left to stand to obtain the liquid product in the lower layer.
为了验证本发明所得到的聚合物具有增稠性能，取2wt. %的聚合物与10wt. %LAS水溶液复配，用NDJ-8S数显粘度仪测得其复配前后的粘度变化，如图2。由图可见，在25℃下，LAS水溶液的粘度基本为零。将本实施例所得的聚合物与LAS复配以后，体系的粘度增加到了1095 mPa·s，证明该聚合物确实有增稠性能。In order to verify that the polymer obtained by the present invention has thickening properties, take 2wt.% polymer and 10wt.% LAS aqueous solution for compounding, and measure the viscosity change before and after its compounding with NDJ-8S digital display viscometer, as shown in Fig. 2. It can be seen from the figure that at 25°C, the viscosity of the LAS aqueous solution is basically zero. After compounding the polymer obtained in this example with LAS, the viscosity of the system increased to 1095 mPa·s, which proves that the polymer does have thickening properties.
实施例6：Embodiment 6:
将脂肪醇聚氧乙烯醚丙烯酸酯30 g、甲基丙烯酸(AA, 8.09 g)溶于去离子水中，加入到装有机械搅拌器、温度计的三口圆底烧瓶中，保持50 ℃搅拌，将0.6 g溴代乙酸乙酯加入到反应体系中，之后升温至150 ℃继续反应1 h。反应结束后，冷却、静置，得到下层液态产物。Dissolve 30 g of fatty alcohol polyoxyethylene ether acrylate and methacrylic acid (AA, 8.09 g) in deionized water, add them into a three-necked round-bottomed flask equipped with a mechanical stirrer and a thermometer, keep stirring at 50 °C, and mix 0.6 One g of ethyl bromoacetate was added to the reaction system, and then the temperature was raised to 150 °C to continue the reaction for 1 h. After the reaction was completed, it was cooled and left to stand to obtain the liquid product in the lower layer.
为了验证本发明所得到的聚合物具有增稠性能，取2wt. %的聚合物与10wt. %LAS水溶液复配，用NDJ-8S数显粘度仪测得其复配前后的粘度变化，如图2。由图可见，在25℃下，LAS水溶液的粘度基本为零。将本实施例所得的聚合物与LAS复配以后，体系的粘度增加到了1195 mPa·s，证明该聚合物确实有增稠性能。In order to verify that the polymer obtained by the present invention has thickening properties, take 2wt.% polymer and 10wt.% LAS aqueous solution for compounding, and measure the viscosity change before and after its compounding with NDJ-8S digital display viscometer, as shown in Fig. 2. It can be seen from the figure that at 25°C, the viscosity of the LAS aqueous solution is basically zero. After compounding the polymer obtained in this example with LAS, the viscosity of the system increased to 1195 mPa·s, which proves that the polymer does have thickening properties.
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| CN117025315A (en) * | 2023-08-11 | 2023-11-10 | 广州立白企业集团有限公司 | Composite thickener and low-active-matter detergent composition containing same |
| CN118852520A (en) * | 2024-06-19 | 2024-10-29 | 广东宏昊化工有限公司 | A nonionic thickener and its preparation method, use, and concentrated laundry detergent |
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