Witconate P-1220EH Calcium dodecylbenzene sulfonate - Nouryon

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发明内容Summary of the invention

为了解决上述技术问题，本发明的第一个方面提供了一种十二烷基苯磺酸钙的制备方法，包括以下步骤：将石粉与促进剂混合均匀，加入十二烷基苯磺酸进行反应，并调节pH至7-8，然后采用板框过滤机除去废渣，滤液经浓缩蒸出高沸点物，剩余产物即为十二烷基苯磺酸钙；其中所述石粉的平均粒径为 0.1mm-12mm。In order to solve the above technical problems, the first aspect of the present invention provides a preparation method of calcium dodecylbenzene sulfonate, comprising the following steps: mixing stone powder and a promoter evenly, adding dodecylbenzene sulfonic acid to react, and adjusting the pH to 7-8, then using a plate and frame filter to remove waste residue, concentrating the filtrate to evaporate high boiling point substances, and the remaining product is calcium dodecylbenzene sulfonate; wherein the average particle size of the stone powder is 0.1mm-12mm.

在一种优选的实施方式中，所述石粉包括第一石粉和第二石粉。所述第一石粉和第二石粉的质量比为1：(2-3)。In a preferred embodiment, the stone powder includes a first stone powder and a second stone powder. The mass ratio of the first stone powder to the second stone powder is 1:(2-3).

在一种优选的实施方式中，所述第一石粉中氧化钙含量≥85wt％。In a preferred embodiment, the calcium oxide content in the first stone powder is ≥ 85wt%.

在一种更优选的实施方式中，所述第一石粉中氧化钙含量为90wt％，氧化镁含量为0.7-2wt％，二氧化硅含量为0.8-1.5wt％。In a more preferred embodiment, the first stone powder contains 90 wt% calcium oxide, 0.7-2 wt% magnesium oxide and 0.8-1.5 wt% silicon dioxide.

在一种优选的实施方式中，所述第一石粉的活性度为350(测试条件： (4mol/mL，40+1，10min)(在40+1℃条件下，用4mol/mL盐酸对石粉进行滴定，第10min时盐酸的用量mL，活性度＝CV/4，C：盐酸浓度，V盐酸体积)。In a preferred embodiment, the activity of the first stone powder is 350 (test conditions: (4 mol/mL, 40+1, 10 min) (at 40+1°C, the stone powder is titrated with 4 mol/mL hydrochloric acid, the amount of hydrochloric acid used at the 10th minute is mL, activity = CV/4, C: hydrochloric acid concentration, V: hydrochloric acid volume).

在一种优选的实施方式中，所述第一石粉的平均粒径为8-12mm。In a preferred embodiment, the average particle size of the first stone powder is 8-12 mm.

在一种优选的实施方式中，所述第二石粉中氢氧化钙含量≥95wt％。In a preferred embodiment, the calcium hydroxide content in the second stone powder is ≥95wt%.

在一种更优选的实施方式中，所述第二石粉中氢氧化钙含量≥95wt％，游离水含量≤1wt％。In a more preferred embodiment, the calcium hydroxide content in the second stone powder is ≥95wt%, and the free water content is ≤1wt%.

在一种优选的实施方式中，所述第二石粉的平均粒径为0.27-0.55mm。In a preferred embodiment, the average particle size of the second stone powder is 0.27-0.55 mm.

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在一种优选的实施方式中，所述促进剂包括二甲苯、甲醇、乙醇、正丁醇、异丁醇、丁二醇、戊醇的至少一种。In a preferred embodiment, the accelerator includes at least one of xylene, methanol, ethanol, n-butanol, isobutanol, butanediol and pentanol.

在一种更优选的实施方式中，所述促进剂包括甲醇。In a more preferred embodiment, the promoter comprises methanol.

在一种优选的实施方式中，所述十二烷基苯磺酸中烷基苯磺含量≥97wt％。In a preferred embodiment, the content of alkylbenzene sulfonate in the dodecylbenzene sulfonic acid is ≥ 97 wt %.

在一种优选的实施方式中，所述促进剂和十二烷基苯磺酸的质量比为 (3.5-4.5)：(0.8-1.2)。In a preferred embodiment, the mass ratio of the accelerator to dodecylbenzenesulfonic acid is (3.5-4.5):(0.8-1.2).

在一种优选的实施方式中，所述石粉和十二烷基苯磺酸的质量比为(0.8-1.2)：(0.8-1.2)。In a preferred embodiment, the mass ratio of the stone powder to dodecylbenzenesulfonic acid is (0.8-1.2): (0.8-1.2).

在一种更优选的实施方式中，所述石粉、促进剂和十二烷基苯磺酸的质量比为1：4：1。In a more preferred embodiment, the mass ratio of the stone powder, the accelerator and dodecylbenzene sulfonic acid is 1:4:1.

在一种优选的实施方式中，所述反应的温度为50-60℃。In a preferred embodiment, the reaction temperature is 50-60°C.

在一种优选的实施方式中，所述反应的时间为3-7h。In a preferred embodiment, the reaction time is 3-7 hours.

本发明的第二个方面提供了一种十二烷基苯磺酸钙，根据如上述的一种十二烷基苯磺酸钙的制备方法制得。The second aspect of the present invention provides calcium dodecylbenzene sulfonate, which is prepared according to the above-mentioned method for preparing calcium dodecylbenzene sulfonate.

有益效果：Beneficial effects:

1)本发明提供了一种十二烷基苯磺酸钙的制备方法，通过对反应过程中原料和反应条件的限定，制备得到的十二烷基苯磺酸钙具有有效成分含量高，水分含量少，收率高，浊度低等优点。1) The present invention provides a method for preparing calcium dodecylbenzene sulfonate. By limiting the raw materials and reaction conditions in the reaction process, the prepared calcium dodecylbenzene sulfonate has the advantages of high content of effective ingredients, low water content, high yield, low turbidity, etc.

2)现有的十二烷基苯磺酸钙制备过程中以纯度较高的碳酸钙、氢氧化钙、氯化钙等为原料，进而提高制备得到的十二烷基苯磺酸钙的收率，但容易造成反应难以控制，水分含量高等缺点。本发明通过采用氧化钙含量为90wt％，氧化镁含量为0.7-2wt％，二氧化硅含量为0.8-1.5wt％，活性度为350，平均粒度为10mm 的第一石粉和氢氧化钙含量≥95wt％，游离水含量≤1wt％第二石粉进行复配，有效控制反应进行的速率，避免部分石粉在反应时间内未充分反应，降低反应速率。尤其是第一石粉和第二石粉的质量比为1：2.5时，制备得到的十二烷基苯磺酸钙有效成分含量高，水分含量低，反应效率高。2) In the existing preparation process of calcium dodecylbenzene sulfonate, calcium carbonate, calcium hydroxide, calcium chloride and the like with high purity are used as raw materials, thereby improving the yield of the prepared calcium dodecylbenzene sulfonate, but it is easy to cause the disadvantages of difficult reaction control and high moisture content. The present invention uses a first stone powder with a calcium oxide content of 90wt%, a magnesium oxide content of 0.7-2wt%, a silicon dioxide content of 0.8-1.5wt%, an activity of 350, and an average particle size of 10mm, and a second stone powder with a calcium hydroxide content of ≥95wt% and a free water content of ≤1wt% to effectively control the reaction rate, avoid partial stone powder from not fully reacting within the reaction time, and reduce the reaction rate. In particular, when the mass ratio of the first stone powder to the second stone powder is 1:2.5, the prepared calcium dodecylbenzene sulfonate has a high content of effective ingredients, a low moisture content, and a high reaction efficiency.

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