CN101880247A - Method for producing naphthalene sulfonic formaldehyde condensation compound - Google Patents
Method for producing naphthalene sulfonic formaldehyde condensation compound Download PDFInfo
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Abstract
The invention relates to a method for producing a naphthalene sulfonic formaldehyde condensation compound. The method solves the technical problems that the method avoids using fuming sulfuric acid and sulfonation entrainer and prepares a product by condensation under low total acidity, and the product does not contain calcium or magnesium ions, has heat-resistant stability and does not produce calcium sulfate waste residue. The method comprises the following steps of: 1) adding washing oil, naphthalene, alkyl naphthalene or benzyl naphthalene serving as a raw material into 96 to 100 percent sulfuric acid, performing sulfonation reaction, and removing water to obtain sulfonation solution, wherein the molar ratio of the raw material to the sulfuric acid is 1: 1.0-1.05; 2) cooling the sulfonation solution, adding water into the solution to adjust the total acidity of the system to between 15 and 19 percent, adding formaldehyde solution into the solution, and performing condensation reaction to obtain the condensation compound, wherein the molar ratio of the sulfonation solution to formaldehyde is 1: 0.6-0.8; and 3) neutralizing the reactants till the pH value is 6 to 9 to obtain a solution product.
Description
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Technical field
The present invention relates to a kind of dyestuff dispersion agent, specifically is a kind of production method of naphthalene sulfonic formaldehyde condensation compound.
Background technology
Dyestuff is raw materials such as washing oil or naphthalene or methylnaphthalene or benzyl naphthalene with the dispersion agent series product synthetic through reactions such as oversulfonate condensations, mainly contain Dispersant MF, dispersion agent NNO, water reducer etc., be that a kind of negatively charged ion shows promoting agent, main dispersion agent and weighting agent as dispersed dye and vat dyes, its consumption accounts for more than 40% of dyestuff commodity.It has mill imitates, and the advantage of polymolecularity, high thermal stability, high temperature good dispersity can be carried out the composite commercialization requirement that has adapted to various dispersed dye and vat dyes with all kinds of dispersion agents of dye well.
Naphthalene is that the production technique of dispersion agent all is with washing oil basically at present, or naphthalene, or methylnaphthalene, or raw material such as benzyl naphthalene, adopt the concentrated acid sulfonation of high mixture ratio, and high total acidity (27 ~ 35%) down and formaldehyde condensation form, vitriolic norm quota of consumption height, contain more excess sulfuric acid in the product, all adopt in the liquid caustic soda and can cause the sodium sulphate content in the product to exceed standard, influence quality product, therefore guaranteeing under the product quality premise, need to use in the lime and the part spent acid, the waste residue that produces a large amount of high COD is difficult for handling, and also introduces calcium ion in the product simultaneously and is difficult for removing.
Patent CN1081451 has introduced a kind of production method of condensation compound of methyl naphthalene sulfonic acid and formaldehyde, it is to adopt the vitriol oil to carry out the azeotropic sulfonation by the entrainer that adds the hexane class in methylnaphthalene, add the condensation material of upward criticizing during condensation and regulate acidity, taking-up part condensation material is waited until down batch condensation and is regulated acidity usefulness after the condensation.Though this method need not adopt in the lime and residual excess acid, need to add entrainer, after finishing, reaction also needs to distill out together the operation of entrainer, also need all to add at every turn and reserve recycle stock, complex process, entrainer are easy to overflow contaminate environment.
Patent CN101386587 has also introduced a kind of production technique of condensation compound of methyl naphthalene sulfonic acid and formaldehyde, and it is to adopt 104.5% oleum to come the sulfonation methylnaphthalene, and then and formaldehyde condensation, use in the liquid caustic soda at last and excessive acid.The sulphonating agent oleum is a kind of high-risk product, and its storage and transportation all have very high requirement, and sulphur trioxide wherein overflows easily, severe contamination storage place and make the environment of use.
Summary of the invention
The technical issues that need to address of the present invention are, avoid using oleum and sulfonation entrainer, adopt the sulfonation of the vitriol oil realization raw material of low proportioning, and condensation prepared naphthalene sulfonic formaldehyde condensation compound product under low total acidity, and not calcic, magnesium ion, heat-resisting stable, do not produce the calcium sulfate waste residue.
The production method of naphthalene sulfonic formaldehyde condensation compound of the present invention comprises the steps:
1) be raw material with washing oil or naphthalene or methylnaphthalene or benzyl naphthalene, it is joined percentage concentration in batches is in 96 ~ 100% the vitriol oil, carries out sulfonation reaction 3 ~ 8 hours under 120 ~ 165 ℃, removes the water that reaction generates by vacuumizing, and obtains sulfonated liquid; Raw material and vitriolic mol ratio are 1:1.0 ~ 1.05;
2) temperature of sulfonated liquid is reduced to 75 ~ 80 ℃, adding water regulation system total acidity is 15 ~ 19%, adds formaldehyde solution, and condensation reaction is 2 ~ 8 hours under 98 ~ 130 ℃, 0 ~ 0.2MPa, obtains condenses; The mol ratio of sulfonated liquid and formaldehyde is 1:0.6 ~ 0.8.
3) after condensation reaction finished, it was 6 ~ 9 that reactant is neutralized to the pH value with sodium hydroxide solution, obtains the solution of naphthalene sulfonic formaldehyde condensation compound.
This method can realize adopting the vitriol oil of equimolar amount to carry out sulfonation substantially, therefore sulfuric acid consumption is by norm than the minimizing of traditional sulfuric acid sulfonation technology about 35%, do not have simultaneously a large amount of like that acid mist of oleum again and produce, fundamentally improve production environment, avoid acid mist effusion contaminate environment.
Factors such as raw materials number of times such as reaction conditions of the present invention and washing oil or naphthalene or methylnaphthalene, reinforced time, each add-on are not made special restriction, only otherwise influencing goal of the invention of the present invention gets final product.The selection that those skilled in the art can more optimize above-mentioned various reaction conditionss and mode by limited experiment according to prior art.As preferably, raw material divides to join for 3 times and carries out sulfonation in the reaction system, adds 65 ~ 75% of the total amount that feeds intake when wherein beginning to feed intake, and sulfonation reaction adds 15 ~ 20% of the total amount that feeds intake again after 1 ~ 3 hour, continue reaction and after 1 ~ 3 hour remaining raw material is added reaction.
This method adopts the sulfuric acid of low proportioning as the sulfonation medium, raw materials such as washing oil or naphthalene or methylnaphthalene or benzyl naphthalene need be joined in batches and carry out sulfonation in the reaction system, to guarantee that raw materials such as washing oil, naphthalene, methylnaphthalene or benzyl naphthalene carry out sulfonation all the time in excessive relatively more sulfuric acid medium, to improve reaction efficiency.The total acidity of system is relatively low in latter stage in sulfonation stage, needs to adopt vacuum system to extract the moisture content that generates in the reaction, impels sulfonation reaction complete, improves sulfonation efficient.
The sulfuric acid sulfonation that adopts low proportioning to terminal after, the system total acidity is lower, can all adopt the liquid caustic soda neutralization with the reaction solution behind the formaldehyde condensation, need be through not filtering, the neutralizer that obtains can directly use through after the spraying drying, has avoided adopting in the traditional technology lime neutralization and a large amount of waste residues of generation.
Dispersion agent of the present invention exists with the form of solid or liquid usually.Wherein can add the various auxiliary agents in some commercial dyes.
The present invention compares with background technology, has that sulfuric acid concentration and consumption are all lower, use is comparatively safe, labour intensity is lower and improves work situation and advantage such as the raw material consumption cost is lower.
Embodiment
Below by embodiment, technical scheme of the present invention is done specific description.Need explanation, protection of the present invention is not limited to this.
Embodiment 1.As follows,
1) in the flask of 1L band prolong, adds the 60g washing oil, be warming up to 90 ℃, slowly drip the 60g vitriol oil (98%), be warming up to 145 ~ 150 ℃ then, add the 15g washing oil again behind the reaction 2h, react adding 10g washing oil after 1 hour again, vacuumize then and continue reaction 1 hour.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 17-18%, adds 36.5% formaldehyde solution 34g.Be warming up to 100 ℃ of insulation reaction 6h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 2.As follows,
1) in the flask of 1L band prolong, adds the 54g naphthalene, be warming up to 80 ℃, slowly drip the 60g vitriol oil (98%), be warming up to 120 ~ 125 ℃ then, add the 13.5g naphthalene again behind the reaction 1h, react adding 9.3g naphthalene after 1 hour again, vacuumize then and continue reaction 1 hour.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 15-16%, adds 36.5% formaldehyde solution 34g.Be warming up to 100 ℃ of insulation reaction 2h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 3.As follows,
1) in the flask of 1L band prolong, adds the 60g methylnaphthalene, be warming up to 80 ℃, slowly drip the 60g vitriol oil (98%), be warming up to 130 ~ 135 ℃ then, add the 15g methylnaphthalene again behind the reaction 2h, react adding 10g methylnaphthalene after 1 hour again, vacuumize then and continue reaction 1 hour.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 16-17%, adds 36.5% formaldehyde solution 34g.Be warming up to 110 ℃ of insulation reaction 5h after adding.
3) in the good material of condensation, add water 90g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 4.As follows,
1) in the flask of 1L band prolong, adds the 92g benzyl naphthalene, be warming up to 80 ℃, slowly drip the 60g vitriol oil (98%), be warming up to 160 ~ 165 ℃ then, add the 23g benzyl naphthalene again behind the reaction 3h, react adding 15.8g benzyl naphthalene after 2 hours again, vacuumize then and continue reaction 3 hours.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 18-19%, adds 36.5% formaldehyde solution 34g.Be warming up to 130 ℃ of insulation reaction 8h after adding.
3) in the good material of condensation, add water 150g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 5.As follows,
1) in the flask of 1L band prolong, adds the 60g washing oil, be warming up to 90 ℃, slowly drip the 63g vitriol oil (98%), be warming up to 145 ~ 150 ℃ then, add the 15g washing oil again behind the reaction 2h, react adding 10g washing oil after 1 hour again, vacuumize then and continue reaction 2 hours.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 18-19%, adds 36.5% formaldehyde solution 34g.Be warming up to 100 ℃ of insulation reaction 5h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 6.As follows,
1) in the flask of 1L band prolong, adds the 60g washing oil, be warming up to 90 ℃, slowly drip the 60g vitriol oil (98%), be warming up to 145 ~ 150 ℃ then, add the 15g washing oil again behind the reaction 2h, react adding 10g washing oil after 1 hour again, vacuumize then and continue reaction 2 hours.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 17-18%, adds 36.5% formaldehyde solution 29.5g.Be warming up to 100 ℃ of insulation reaction 3h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 7.As follows,
1) in the flask of 1L band prolong, adds the 60g washing oil, be warming up to 90 ℃, slowly drip the 62g vitriol oil (98%), be warming up to 145 ~ 150 ℃ then, add the 15g washing oil again behind the reaction 2h, react adding 10g washing oil after 1 hour again, vacuumize then and continue reaction 2 hours.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 17-18%, adds 36.5% formaldehyde solution 38g.Be warming up to 110 ℃ of insulation reaction 4h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 8.As follows,
1) in the flask of 1L band prolong, adds the 55g washing oil, be warming up to 90 ℃, slowly drip the 64g vitriol oil (96%), be warming up to 145 ~ 150 ℃ then, add the 17g washing oil again behind the reaction 2h, react adding 13g washing oil after 1 hour again, vacuumize then and continue reaction 2 hours.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 16-17%, adds 36.5% formaldehyde solution 34g.Be warming up to 100 ℃ of insulation reaction 6h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Embodiment 9.As follows,
1) in the flask of 1L band prolong, adds the 63g washing oil, be warming up to 90 ℃, slowly drip the 60g vitriol oil (100%), be warming up to 145 ~ 150 ℃ then, add the 16g washing oil again behind the reaction 2h, react adding 6g washing oil after 1 hour again, vacuumize then and continue reaction 1 hour.
2) sulfonation is good material is cooled to 100 ℃, adds suitable quantity of water and regulates the material total acidity to 17-18%, adds 36.5% formaldehyde solution 34g.Be warming up to 100 ℃ of insulation reaction 6h after adding.
3) in the good material of condensation, add water 100g, add 30% liquid caustic soda simultaneously and regulate material pH value 6 ~ 9, obtain the dispersion agent finished fluid, obtain the finished product powder after spray is dried, solid content 37 ~ 42%, thermostability 〉=135 ℃.
Claims (2)
1. the production method of a naphthalene sulfonic formaldehyde condensation compound comprises the steps:
1) be raw material with washing oil or naphthalene or methylnaphthalene or benzyl naphthalene, it is joined percentage concentration is in 96 ~ 100% the vitriol oil, carries out sulfonation reaction 3 ~ 8 hours under 120 ~ 165 ℃, removes the water that reaction generates by vacuumizing, and obtains sulfonated liquid; Raw material and vitriolic mol ratio are 1:1.0 ~ 1.05;
2) temperature of sulfonated liquid is reduced to 75 ~ 80 ℃, adding water regulation system total acidity is 15 ~ 19%, adds formaldehyde solution, and condensation reaction is 2 ~ 8 hours under 98 ~ 130 ℃, 0 ~ 0.2MPa, obtains condenses; The mol ratio of sulfonated liquid and formaldehyde is 1:0.6 ~ 0.8;
3) after condensation reaction finished, it was 6 ~ 9 that reactant is neutralized to the pH value with sodium hydroxide solution, obtains the solution of naphthalene sulfonic formaldehyde condensation compound.
2. the production method of naphthalene sulfonic formaldehyde condensation compound according to claim 1, it is characterized in that raw material divides to join for 3 times carries out sulfonation in the reaction system, add 65 ~ 75% of the total amount that feeds intake when wherein beginning to feed intake, sulfonation reaction adds 15 ~ 20% of the total amount that feeds intake again after 1 ~ 3 hour, continue reaction and after 1 ~ 3 hour remaining raw material is added reaction.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102250655A (en) * | 2011-06-10 | 2011-11-23 | 天津市双盛化学助剂工贸有限公司 | Preparation method of high-fluidity gasified water-coal slurry dispersant |
| CN102746195A (en) * | 2011-04-27 | 2012-10-24 | 江苏尼高科技有限公司 | Method for improving sulfonation process of naphthalene-based water reducer |
| CN103524385A (en) * | 2013-10-15 | 2014-01-22 | 浙江秦燕化工有限公司 | Preparation method for modified disperse dye dispersing agent and product |
| CN103613519A (en) * | 2013-12-06 | 2014-03-05 | 安阳市双环助剂有限责任公司 | Production method for dispersing agent XY |
| CN103664710A (en) * | 2013-12-26 | 2014-03-26 | 浙江闰土研究院有限公司 | Preparation method of quinoline-free dispersing agent |
| CN104479405A (en) * | 2014-11-24 | 2015-04-01 | 江阴市盛通化工有限公司 | High-temperature-resistant mixed dispersant NNO/MF and production process thereof |
| CN105566170A (en) * | 2016-01-22 | 2016-05-11 | 绍兴文理学院 | Recycling method for dilute sulphuric acid |
| CN105712906A (en) * | 2016-03-29 | 2016-06-29 | 绍兴文理学院 | Method for preparing high-quality dispersing agent MF with reactive distillation method |
| CN107602421A (en) * | 2017-08-24 | 2018-01-19 | 南通双狮化工有限公司 | A kind of preparation technology of naphthalene sulfonic acids and butyl naphthalene sulfonic acid-formaldehyde condensation product |
| CN107674005A (en) * | 2017-08-24 | 2018-02-09 | 南通双狮化工有限公司 | A kind of preparation method of high-concentration naphthalene sulfonic acid formaldehyde condensation products |
| CN107739320A (en) * | 2017-08-24 | 2018-02-27 | 南通双狮化工有限公司 | A kind of preparation method of naphthalene sulfonic acid-formaldehyde condensation product |
| CN109020843A (en) * | 2018-09-20 | 2018-12-18 | 江苏精禾界面科技有限公司 | A kind of naphthalene sulfonate-alkylnaphthalene sulfonate-formaldehyde condensation products preparation method and applications |
| CN109096153A (en) * | 2018-09-18 | 2018-12-28 | 江苏精禾界面科技有限公司 | A kind of continuous flow prepares the new method of naphthalene sulfonic sodium formaldehyde condensation product |
| CN109574885A (en) * | 2018-10-25 | 2019-04-05 | 浙江龙盛化工研究有限公司 | A kind of preparation method of low contamination Dispersant MF |
| CN110256303A (en) * | 2019-07-05 | 2019-09-20 | 浙江闰土研究院有限公司 | Dispersant MF and preparation method thereof |
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| CN102746195A (en) * | 2011-04-27 | 2012-10-24 | 江苏尼高科技有限公司 | Method for improving sulfonation process of naphthalene-based water reducer |
| CN102250655A (en) * | 2011-06-10 | 2011-11-23 | 天津市双盛化学助剂工贸有限公司 | Preparation method of high-fluidity gasified water-coal slurry dispersant |
| CN103524385A (en) * | 2013-10-15 | 2014-01-22 | 浙江秦燕化工有限公司 | Preparation method for modified disperse dye dispersing agent and product |
| CN103524385B (en) * | 2013-10-15 | 2015-04-29 | 浙江秦燕化工有限公司 | Preparation method for modified disperse dye dispersing agent and product |
| CN103613519A (en) * | 2013-12-06 | 2014-03-05 | 安阳市双环助剂有限责任公司 | Production method for dispersing agent XY |
| CN103664710B (en) * | 2013-12-26 | 2015-09-23 | 浙江闰土研究院有限公司 | A kind of preparation method without quinoline dispersion agent |
| CN103664710A (en) * | 2013-12-26 | 2014-03-26 | 浙江闰土研究院有限公司 | Preparation method of quinoline-free dispersing agent |
| CN104479405B (en) * | 2014-11-24 | 2017-01-18 | 江阴市盛通化工有限公司 | High-temperature-resistant mixed dispersant NNO/MF and production process thereof |
| CN104479405A (en) * | 2014-11-24 | 2015-04-01 | 江阴市盛通化工有限公司 | High-temperature-resistant mixed dispersant NNO/MF and production process thereof |
| CN105566170A (en) * | 2016-01-22 | 2016-05-11 | 绍兴文理学院 | Recycling method for dilute sulphuric acid |
| CN105712906A (en) * | 2016-03-29 | 2016-06-29 | 绍兴文理学院 | Method for preparing high-quality dispersing agent MF with reactive distillation method |
| CN105712906B (en) * | 2016-03-29 | 2017-10-10 | 绍兴文理学院 | A kind of method that reaction rectification method prepares high-quality Dispersant MF |
| CN107739320A (en) * | 2017-08-24 | 2018-02-27 | 南通双狮化工有限公司 | A kind of preparation method of naphthalene sulfonic acid-formaldehyde condensation product |
| CN107674005A (en) * | 2017-08-24 | 2018-02-09 | 南通双狮化工有限公司 | A kind of preparation method of high-concentration naphthalene sulfonic acid formaldehyde condensation products |
| CN107602421A (en) * | 2017-08-24 | 2018-01-19 | 南通双狮化工有限公司 | A kind of preparation technology of naphthalene sulfonic acids and butyl naphthalene sulfonic acid-formaldehyde condensation product |
| CN109096153A (en) * | 2018-09-18 | 2018-12-28 | 江苏精禾界面科技有限公司 | A kind of continuous flow prepares the new method of naphthalene sulfonic sodium formaldehyde condensation product |
| CN109096153B (en) * | 2018-09-18 | 2021-01-12 | 江苏精禾界面科技有限公司 | New method for preparing naphthalene series sodium sulfonate formaldehyde condensate by continuous flow |
| CN109020843A (en) * | 2018-09-20 | 2018-12-18 | 江苏精禾界面科技有限公司 | A kind of naphthalene sulfonate-alkylnaphthalene sulfonate-formaldehyde condensation products preparation method and applications |
| CN109574885A (en) * | 2018-10-25 | 2019-04-05 | 浙江龙盛化工研究有限公司 | A kind of preparation method of low contamination Dispersant MF |
| CN109574885B (en) * | 2018-10-25 | 2021-10-08 | 浙江龙盛化工研究有限公司 | Preparation method of low-contamination dispersant MF |
| CN110256303A (en) * | 2019-07-05 | 2019-09-20 | 浙江闰土研究院有限公司 | Dispersant MF and preparation method thereof |
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Application publication date: 20101110 |