CN112210227B - Cationic golden dye and preparation method thereof - Google Patents
Cationic golden dye and preparation method thereof Download PDFInfo
- Publication number
- CN112210227B CN112210227B CN201910618195.9A CN201910618195A CN112210227B CN 112210227 B CN112210227 B CN 112210227B CN 201910618195 A CN201910618195 A CN 201910618195A CN 112210227 B CN112210227 B CN 112210227B
- Authority
- CN
- China
- Prior art keywords
- golden yellow
- dimethyl sulfate
- reaction
- water
- filtrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 125000002091 cationic group Chemical group 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 claims abstract description 40
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000047 product Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims abstract 4
- -1 hydroxyl golden yellow Chemical compound 0.000 claims abstract 3
- 238000004321 preservation Methods 0.000 claims abstract 2
- 239000002243 precursor Substances 0.000 claims description 22
- 238000005292 vacuum distillation Methods 0.000 claims description 9
- 239000001043 yellow dye Substances 0.000 claims description 7
- 239000013505 freshwater Substances 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 239000002904 solvent Substances 0.000 abstract description 7
- 239000002351 wastewater Substances 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000012022 methylating agents Substances 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 9
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000012805 post-processing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000001035 methylating effect Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B26/00—Hydrazone dyes; Triazene dyes
- C09B26/02—Hydrazone dyes
- C09B26/04—Hydrazone dyes cationic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
技术领域technical field
本发明涉及一种阳离子金黄染料及其制备方法，属于染料技术领域。The invention relates to a cationic golden yellow dye and a preparation method thereof, belonging to the technical field of dyes.
背景技术Background technique
目前金黄-28合成工艺为以金黄-28母体为起始原料、硫酸二甲酯为甲基化试剂、二氯乙烷为溶剂、氧化镁或碳酸钠为缚酸剂在回流温度(70～75℃)下进行，所得产品为硫酸单甲酯根的阳离子金黄-28染料原粉。At present, the synthesis process of Jinhuang-28 is to use Jinhuang-28 parent as starting material, dimethyl sulfate as methylating reagent, dichloroethane as solvent, magnesium oxide or sodium carbonate as acid binding agent at reflux temperature (70～75 ℃), the resulting product is the cationic golden yellow-28 dye original powder of monomethyl sulfate.
目前工艺技术的缺点：(1)所用原料金黄母体为潮品，含水率较高(40％左右)，从而使得甲基化试剂硫酸二甲酯需大过量(过量120％)，从而使增加生产成本，且会增加工艺废水的COD进一步增加废水处理成本；(2)目前工艺所用缚酸剂氧化镁微溶于水不溶于有机溶剂，缚酸效果不佳且会增加后处理成本。缚酸剂碳酸钠缚酸效果较好，但其会增加工艺废水的盐分含量同样会增加废水处理成本。Disadvantages of the current technology: (1) The used raw material golden yellow precursor is a wet product with a high water content (about 40%), so that the methylating reagent dimethyl sulfate needs to be excessively (excessive 120%), thereby increasing the production. (2) The acid binding agent magnesium oxide used in the current process is slightly soluble in water and insoluble in organic solvents, and the acid binding effect is not good and will increase the post-treatment cost. The acid binding agent sodium carbonate has better acid binding effect, but it will increase the salt content of the process wastewater and also increase the cost of wastewater treatment.
针对目前工艺技术的缺点，主要是降低甲基化试剂硫酸二甲酯的用量以降低生产成本，选择效果优良的缚酸剂降低工艺废水产生量及其处理成本。In view of the shortcomings of the current process technology, the main purpose is to reduce the amount of methylation reagent dimethyl sulfate to reduce production costs, and to select acid binding agents with excellent effects to reduce process wastewater production and treatment costs.
发明内容SUMMARY OF THE INVENTION
有鉴于此，本发明提供了一种阳离子金黄染料及其制备方法，取消了生产溶剂的使用，降低了产品的生产成本；降低了工艺废水的产生量，进一步降低了产品的生产成本；过量甲基化试剂可回收套用；后处理用水亦可回收套用，降低三废处理成本。In view of this, the present invention provides a cationic golden yellow dye and a preparation method thereof, which eliminates the use of production solvent, reduces the production cost of the product; reduces the production amount of process wastewater, and further reduces the production cost of the product; The base reagent can be recycled and applied; the post-treatment water can also be recycled and applied to reduce the cost of three wastes treatment.
本发明通过以下技术手段解决上述技术问题：The present invention solves the above-mentioned technical problems through the following technical means:
本发明的一种阳离子金黄染料及其制备方法，将金黄母体干品、缚酸剂氢氧根金黄原粉投入反应瓶中，继续投入硫酸二甲酯，然后快速升温至75～90℃，保温反应8～60min，反应完毕后减压蒸馏回收过量的硫酸二甲酯进行套用，剩余物料加水后在60～65℃下搅拌30min后降温至20℃以下进行过滤、干燥后即得硫酸甲酯根的金黄-28原粉，滤液可以套用于下一批的后处理操作。In the cationic golden yellow dye and the preparation method thereof of the present invention, the dry product of golden yellow precursor and the acid binding agent hydroxide golden yellow original powder are put into a reaction flask, continue to be put into dimethyl sulfate, and then rapidly heated to 75-90 DEG C, and the temperature is kept warm. The reaction is carried out for 8-60 min. After the reaction is completed, the excess dimethyl sulfate is recovered by distillation under reduced pressure and applied mechanically. After adding water to the remaining material, the mixture is stirred at 60-65 ° C for 30 min, cooled to below 20 ° C, filtered, and dried to obtain methyl sulfate radical. The filtrate can be used for the next batch of post-processing operations.
所述金黄母体干品、缚酸剂氢氧根金黄原粉摩尔比为1:0.2～0.8。The molar ratio of the dried golden yellow precursor and the acid binding agent hydroxide golden yellow original powder is 1:0.2-0.8.
所述硫酸二甲酯加入的摩尔数为金黄母体摩尔数的4～8倍。The mole number of the dimethyl sulfate added is 4 to 8 times the mole number of the golden yellow precursor.
加入的水为金黄母体干品质量的4倍。The added water is 4 times the mass of the dry product of the golden precursor.
金黄母体干品的水分含量小于5％。The moisture content of the dried golden yellow precursor is less than 5%.
将滤液经减压蒸馏回收硫酸二甲酯后所得剩余物料加入水升温至60～65℃下搅拌30min后降温至20℃以下进行过滤，所得滤液当作下一批后处理所需水，不足量用新鲜水补齐。After the filtrate is distilled under reduced pressure to recover the dimethyl sulfate, the remaining material is added with water, and the temperature is raised to 60 to 65 ° C and stirred for 30 minutes, and then cooled to below 20 ° C for filtration. Top up with fresh water.
减压蒸馏时的工艺条件为：压力为-0.1MPa，温度为125～130℃The process conditions during vacuum distillation are: the pressure is -0.1MPa, and the temperature is 125～130℃
本发明将原料金黄母体潮品改为金黄母体干品(水分含量小于5％)；(2)去除专用溶剂二氯乙烷，将硫酸二甲酯同时做甲基化试剂及溶剂，反应完毕后过量的硫酸二甲酯可以回收重复使用；(3)缚酸剂改为氢氧根的金黄原粉干品(有机碱)，在过量硫酸二甲酯体系中最终都转化为硫酸甲酯根产品，无废物产生，整个工艺过程产生的废水量大大降低；(4)反应温度较为温和(75～90℃)，反应时间较短(8～10min)，反应速度较快，较为适用于管道反应生产方式。In the present invention, the wet product of the raw golden yellow precursor is changed to a dry product of the golden yellow precursor (the moisture content is less than 5%); (2) the special solvent dichloroethane is removed, and dimethyl sulfate is used as a methylating reagent and a solvent at the same time, and after the reaction is completed Excessive dimethyl sulfate can be recovered and reused; (3) acid binding agent is changed into the dry product (organic alkali) of the golden yellow original powder of hydroxide, which is finally converted into methyl sulfate product in the excess dimethyl sulfate system , no waste is generated, and the amount of wastewater generated in the whole process is greatly reduced; (4) the reaction temperature is relatively mild (75 ~ 90 ℃), the reaction time is short (8 ~ 10min), and the reaction speed is relatively fast, which is more suitable for pipeline reaction production Way.
滤液可当做下一批进行后处理得水进行循环套用，从而减少工艺废水的产生。具体操作方法为：将上一批经减压蒸馏回收硫酸二甲酯后所得剩余物料加入水升温至60～65℃下搅拌30min后降温至20℃以下进行过滤，所得滤液当作下一批后处理所需水(不足量用新鲜水补齐)，以减少废水量的产生，进而降低产品的工艺成本。减压蒸馏又称真空蒸馏是分离和提纯化合物的一种重要方法，尤其适用于高沸点物质和那些在常压蒸馏时未达到沸点就已受热分解、氧化或聚合的化合物的分离和提纯。The filtrate can be recycled as the next batch of post-treated water, thereby reducing the production of process wastewater. The specific operation method is as follows: adding the remaining material obtained after the recovery of dimethyl sulfate by distillation under reduced pressure in the previous batch, adding water and heating to 60-65 °C, stirring for 30 minutes, then cooling to below 20 °C for filtration, and the obtained filtrate is treated as the next batch. Treat the required water (the insufficient amount is filled with fresh water) to reduce the generation of waste water, thereby reducing the process cost of the product. Vacuum distillation, also known as vacuum distillation, is an important method for separating and purifying compounds, especially for the separation and purification of high-boiling substances and those compounds that have been thermally decomposed, oxidized or polymerized before reaching the boiling point during atmospheric distillation.
化合物的沸点总是随外界压力的不同而变化，某些沸点较高的(尤其200℃以上)的化合物在常压下蒸馏时，由于温度的升高，未达到沸点时往往发生分解、氧化或聚合等现象。此时，不能用常压蒸馏，而应使用减压蒸馏。通过减少体系内的压力而降低液体的沸点，从而避免这些现象的发生。The boiling point of the compound always changes with the external pressure. When some compounds with a higher boiling point (especially above 200°C) are distilled under normal pressure, due to the increase of temperature, decomposition, oxidation or decomposition occurs before the boiling point is reached. aggregation, etc. At this time, atmospheric distillation cannot be used, but reduced pressure distillation should be used. These phenomena are avoided by reducing the pressure in the system to lower the boiling point of the liquid.
本发明中所用到的硫酸二甲酯在常压下沸点为188℃，且在其沸点温度时该化合物易分解，而该发明中过量的硫酸二甲酯要达到回收再利用降低工艺成本的目的只能使用减压蒸馏的方法使其与产品在较低温度下得到有效分离，其具体方法是通过真空泵抽真空降低反应混合物体系的压力，从而达到降低所需回收的过量硫酸二甲酯的沸点，然后在较低压力下对其进行蒸馏回收操作使其在较低温度下与产品得到有效分离，从而实现过量硫酸二甲酯的回收再利用进而降低生产工艺成本。具体减压蒸馏时的工艺条件为：-0.1MPa，125～130℃。The dimethyl sulfate used in the present invention has a boiling point of 188° C. under normal pressure, and the compound is easily decomposed at its boiling temperature, and the excess dimethyl sulfate in the present invention is to achieve the purpose of recycling and reducing process costs. Only the method of vacuum distillation can be used to effectively separate it from the product at a lower temperature, and its specific method is to reduce the pressure of the reaction mixture system through vacuum pumping, so as to reduce the boiling point of the excess dimethyl sulfate that needs to be recovered. , and then carry out a distillation recovery operation at a lower pressure to effectively separate it from the product at a lower temperature, thereby realizing the recovery and reuse of the excess dimethyl sulfate and reducing the production process cost. The specific process conditions during vacuum distillation are: -0.1MPa, 125-130°C.
本发明的有益效果：(1)取消了溶剂的使用，利用过量的硫酸二甲酯既做反应物又做溶剂且可回收套用；(2)缚酸剂的选择使用产品的不同阴离子(氢氧根离子)碱替代，无废物产生；(3)反应时间较短，反应速度较快，适合应用于管道化生产方式；(4)三废产生量大大降低，降低产品的生产成本。Beneficial effects of the present invention: (1) the use of solvent is cancelled, and excess dimethyl sulfate is used as both a reactant and a solvent and can be recycled and applied; (2) the selection of acid binding agent uses different anions (hydrogen oxygen) of the product (3) The reaction time is short and the reaction speed is fast, which is suitable for pipeline production; (4) The production of three wastes is greatly reduced, and the production cost of the product is reduced.
具体实施方式Detailed ways
以下将结合具体实施例对本发明进行详细说明，本实施例的一种阳离子金黄染料及其制备方法，将金黄母体干品、缚酸剂氢氧根金黄原粉投入反应瓶中，继续投入硫酸二甲酯，然后快速升温至75～90℃，保温反应8～60min，反应完毕后减压蒸馏回收过量的硫酸二甲酯进行套用，剩余物料加水后在60～65℃下搅拌30min后降温至20℃以下进行过滤、干燥后即得硫酸甲酯根的金黄-28原粉，滤液可以套用于下一批的后处理操作。The present invention will be described in detail below with reference to specific embodiments. A cationic golden yellow dye and a preparation method thereof of the present embodiment are as follows: the dry product of golden yellow precursor and acid binding agent hydroxide golden yellow original powder are put into the reaction flask, and the sulfuric acid dichloride is continuously added. The methyl ester is then rapidly heated to 75 to 90°C, and the reaction is incubated for 8 to 60 minutes. After the reaction is completed, excess dimethyl sulfate is recovered by distillation under reduced pressure for mechanical application. After adding water to the remaining material, the mixture is stirred at 60 to 65°C for 30 minutes and then cooled to 20°C. After filtration and drying below ℃, the golden yellow-28 original powder of methyl sulfate radical is obtained, and the filtrate can be applied to the next batch of post-processing operations.
所述金黄母体干品、缚酸剂氢氧根金黄原粉摩尔比为1:0.2～0.8。The molar ratio of the dried golden yellow precursor and the acid binding agent hydroxide golden yellow original powder is 1:0.2-0.8.
所述硫酸二甲酯加入的摩尔数为金黄母体摩尔数的4～8倍。The mole number of the dimethyl sulfate added is 4 to 8 times the mole number of the golden yellow precursor.
加入的水为金黄母体干品质量的4倍。The added water is 4 times the mass of the dry product of the golden precursor.
金黄母体干品的水分含量小于5％。The moisture content of the dried golden yellow precursor is less than 5%.
将滤液经减压蒸馏回收硫酸二甲酯后所得剩余物料加入水升温至60～65℃下搅拌30min后降温至20℃以下进行过滤，所得滤液当作下一批后处理所需水，不足量用新鲜水补齐。After the filtrate is distilled under reduced pressure to recover the dimethyl sulfate, the remaining material is added with water, and the temperature is raised to 60 to 65 ° C and stirred for 30 minutes, and then cooled to below 20 ° C for filtration. Top up with fresh water.
减压蒸馏时的工艺条件为：压力为-0.1MPa，温度为125～130℃。The process conditions during the vacuum distillation are: the pressure is -0.1MPa, and the temperature is 125-130°C.
实施例1Example 1
一种阳离子金黄染料及其制备方法，将金黄母体干品、缚酸剂氢氧根金黄原粉投入反应瓶中，继续投入硫酸二甲酯，然后快速升温至86℃，保温反应30min，反应完毕后减压蒸馏回收过量的硫酸二甲酯进行套用，剩余物料加水后在63℃下搅拌30min后降温至20℃以下进行过滤、干燥后即得硫酸甲酯根的金黄-28原粉，滤液可以套用于下一批的后处理操作。A cationic golden yellow dye and a preparation method thereof. The golden yellow precursor dry product and the acid binding agent hydroxide golden yellow original powder are put into a reaction flask, continue to be put into dimethyl sulfate, and then rapidly heated to 86° C., and the reaction is maintained for 30 minutes, and the reaction is completed. The excess dimethyl sulfate was recovered by distillation under reduced pressure and applied mechanically. After adding water to the remaining material, stirring at 63° C. for 30 min, the temperature was lowered to below 20° C. for filtration and drying to obtain the original powder of methyl sulfate radical-28. The filtrate can be Apply to the next batch of post-processing operations.
所述金黄母体干品、缚酸剂氢氧根金黄原粉摩尔比为1:0.6。The dry product of the golden yellow precursor and the acid binding agent hydroxide golden yellow original powder have a molar ratio of 1:0.6.
所述硫酸二甲酯加入的摩尔数为金黄母体摩尔数的7倍。The moles of the dimethyl sulfate added are 7 times the moles of the golden yellow parent.
加入的水为金黄母体干品质量的4倍。The added water is 4 times the mass of the dry product of the golden precursor.
金黄母体干品的水分含量小于5％。The moisture content of the dried golden yellow precursor is less than 5%.
将滤液经减压蒸馏回收硫酸二甲酯后所得剩余物料加入水升温至63℃下搅拌30min后降温至20℃以下进行过滤，所得滤液当作下一批后处理所需水，不足量用新鲜水补齐。After the filtrate was distilled under reduced pressure to recover the dimethyl sulfate, the remaining material was added with water and heated to 63°C and stirred for 30min, and then cooled to below 20°C for filtration. Fill up with water.
减压蒸馏时的工艺条件为：压力为-0.1MPa，温度为128℃。The process conditions during the vacuum distillation were as follows: the pressure was -0.1MPa, and the temperature was 128°C.
实施例2Example 2
一种阳离子金黄染料及其制备方法，将金黄母体干品、缚酸剂氢氧根金黄原粉投入反应瓶中，继续投入硫酸二甲酯，然后快速升温至80℃，保温反应50min，反应完毕后减压蒸馏回收过量的硫酸二甲酯进行套用，剩余物料加水后在65℃下搅拌30min后降温至20℃以下进行过滤、干燥后即得硫酸甲酯根的金黄-28原粉，滤液可以套用于下一批的后处理操作。A cationic golden yellow dye and a preparation method thereof. The dry product of golden yellow precursor and the acid-binding agent hydroxide golden yellow original powder are put into a reaction flask, dimethyl sulfate is continuously added, and then the temperature is rapidly raised to 80° C., and the reaction is kept for 50 minutes, and the reaction is completed. The excess dimethyl sulfate was recovered by distillation under reduced pressure and applied mechanically. After adding water to the remaining material, stirring at 65 ° C for 30 min, the temperature was lowered to below 20 ° C for filtration and drying to obtain the original powder of methyl sulfate radical-28. The filtrate can be Apply to the next batch of post-processing operations.
所述金黄母体干品、缚酸剂氢氧根金黄原粉摩尔比为1:0.5。The dry product of the golden yellow precursor and the acid binding agent hydroxide golden yellow original powder have a molar ratio of 1:0.5.
所述硫酸二甲酯加入的摩尔数为金黄母体摩尔数的7倍。The moles of the dimethyl sulfate added are 7 times the moles of the golden yellow parent.
加入的水为金黄母体干品质量的4倍。The added water is 4 times the mass of the dry product of the golden precursor.
金黄母体干品的水分含量小于5％。The moisture content of the dried golden yellow precursor is less than 5%.
将滤液经减压蒸馏回收硫酸二甲酯后所得剩余物料加入水升温至65℃下搅拌30min后降温至20℃以下进行过滤，所得滤液当作下一批后处理所需水，不足量用新鲜水补齐。After the filtrate is distilled under reduced pressure to recover the dimethyl sulfate, the remaining material obtained is added with water and heated to 65 ° C and stirred for 30 min, and then cooled to below 20 ° C for filtration. Fill up with water.
减压蒸馏时的工艺条件为：压力为-0.1MPa，温度为125℃。The process conditions during the vacuum distillation were: the pressure was -0.1MPa, and the temperature was 125°C.
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be Modifications or equivalent replacements without departing from the spirit and scope of the technical solutions of the present invention should be included in the scope of the claims of the present invention.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910618195.9A CN112210227B (en) | 2019-07-10 | 2019-07-10 | Cationic golden dye and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910618195.9A CN112210227B (en) | 2019-07-10 | 2019-07-10 | Cationic golden dye and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112210227A CN112210227A (en) | 2021-01-12 |
| CN112210227B true CN112210227B (en) | 2022-06-10 |
Family
ID=74047420
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910618195.9A Active CN112210227B (en) | 2019-07-10 | 2019-07-10 | Cationic golden dye and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112210227B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0229980A2 (en) * | 1985-12-21 | 1987-07-29 | Bayer Ag | Process for the manufacture of cationic hydrazone dyes |
| JP2001019866A (en) * | 1999-07-08 | 2001-01-23 | Orient Chem Ind Ltd | Preparation of azamethine salt-forming substance dye, and oil-soluble dye ink |
| CN1667050A (en) * | 2004-03-10 | 2005-09-14 | 杭州近江化工染料有限公司 | Method for preparing high concentration liquid cationic dyes |
| CN1743383A (en) * | 2004-09-01 | 2006-03-08 | 上海汇友精密化学品有限公司 | A new process for quaternization of cationic dye precursors |
| CN101245195A (en) * | 2008-03-14 | 2008-08-20 | 上海富圆染化有限公司 | A kind of novel heterocyclic azo cationic dye and preparation method thereof |
| CN101724290A (en) * | 2009-12-10 | 2010-06-09 | 杭州璟江瑞华科技有限公司 | Preparation method of environment-friendly zinc-free cationic dye |
| CN105417815A (en) * | 2015-11-06 | 2016-03-23 | 南京师范大学 | Method for treating salt-containing organic wastewater during production of cationic golden yellow dye X-GL |
-
2019
- 2019-07-10 CN CN201910618195.9A patent/CN112210227B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0229980A2 (en) * | 1985-12-21 | 1987-07-29 | Bayer Ag | Process for the manufacture of cationic hydrazone dyes |
| JP2001019866A (en) * | 1999-07-08 | 2001-01-23 | Orient Chem Ind Ltd | Preparation of azamethine salt-forming substance dye, and oil-soluble dye ink |
| CN1667050A (en) * | 2004-03-10 | 2005-09-14 | 杭州近江化工染料有限公司 | Method for preparing high concentration liquid cationic dyes |
| CN1743383A (en) * | 2004-09-01 | 2006-03-08 | 上海汇友精密化学品有限公司 | A new process for quaternization of cationic dye precursors |
| CN101245195A (en) * | 2008-03-14 | 2008-08-20 | 上海富圆染化有限公司 | A kind of novel heterocyclic azo cationic dye and preparation method thereof |
| CN101724290A (en) * | 2009-12-10 | 2010-06-09 | 杭州璟江瑞华科技有限公司 | Preparation method of environment-friendly zinc-free cationic dye |
| CN105417815A (en) * | 2015-11-06 | 2016-03-23 | 南京师范大学 | Method for treating salt-containing organic wastewater during production of cationic golden yellow dye X-GL |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112210227A (en) | 2021-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109336831B (en) | Method for recovering triazine ring from triazine ring wastewater | |
| CN102229586A (en) | Preparation method for alpha-acetyl-gamma-butyrolactone | |
| CN103058845A (en) | Dibenzoylmethane preparation method | |
| CN106810450A (en) | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate | |
| CN101402899A (en) | Oxidization fine purification albefaction method for montan wax | |
| CN106006676B (en) | A kind of method of NaOH in recovery H soda acid process of smelting | |
| CN115894229B (en) | Selective synthesis process of adipic acid monoethyl ester | |
| CN112210227B (en) | Cationic golden dye and preparation method thereof | |
| CN105175353B (en) | The method of ammonolysis dioxygen oxidation synthetic rubber accelerant MBT | |
| CN106495174A (en) | Attapulgite wet method bisgallic acid activation method | |
| KR20180016425A (en) | Improved Process for Making Diaryl Sulfones | |
| CN104829595A (en) | Novel technology for preparing esomeprazole sodium by employing chiral porphyrin catalytic oxidation | |
| CN104151251A (en) | Method for one-pot synthesis of 5-acetylacetamido-benzimidazolone | |
| CN109503343B (en) | Preparation method of photoinitiator 184 | |
| CN104058936A (en) | Method for separation and purification of p-cresol | |
| CN107473927B (en) | Preparation process of biphenyl dichlorobenzyl | |
| CN105330545A (en) | Method for recycling oxalic acid from triazine ring cyclization mother liquor dreg with tin chloride as catalyst | |
| CN105753659B (en) | A kind of method that lignin oxidation's degraded prepares vanillyl alcohol | |
| CN115974304A (en) | A treatment device and treatment method for sodium bromide wastewater in the production process of photoinitiator | |
| CN103980105A (en) | Method for preparing p-methoxybenzaldehyde by p-methoxybenzoic acid | |
| CN103319318A (en) | Recovering and recycling method of excessive methyl catechol in vanillin production process | |
| JP2019529412A (en) | Methanol and acetone removal unit, and phenol and bisphenol A production system including the same | |
| CN106986762A (en) | A kind of technique for preparing DL mandelic acids | |
| CN103772153B (en) | Synthetic method and system of 4-chloro-3-cresol | |
| CN109485070B (en) | A kind of method for processing triazine ring sodium salt mother liquor slag |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |