CN103450055A - Preparation method of improved sulfosuccinate penetrant - Google Patents
Preparation method of improved sulfosuccinate penetrant Download PDFInfo
- Publication number
- CN103450055A CN103450055A CN2012101764117A CN201210176411A CN103450055A CN 103450055 A CN103450055 A CN 103450055A CN 2012101764117 A CN2012101764117 A CN 2012101764117A CN 201210176411 A CN201210176411 A CN 201210176411A CN 103450055 A CN103450055 A CN 103450055A
- Authority
- CN
- China
- Prior art keywords
- penetrant
- preparation
- sulfosuccinate
- improved
- permeate agent
- 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.)
- Pending
Links
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a preparation method of an improved sulfosuccinate penetrant. The preparation method is designed based on the traditional penetrant production method, utilizes a novel composite acid as a catalyst, shortens reaction time, and solves the problem that the traditional sulfosuccinate penetrant has a low sulfonation conversion rate and unstable penetration effects. The preparation method of the improved sulfosuccinate penetrant has the advantages of simple processes, low production cost, good skin compatibility, small irritation, bio-safety, easy degradation, and no three-waste pollution according with safe and environmentally friendly new concepts, has high surface activity, and can be used in fields of weaving, printing and dyeing, papermaking, pesticide, washing, medicine and cosmetic.
Description
What the present invention relates to is a kind of process of preparing of modified form succinin sulfonate permeate agent.
Amber acid ester sulfonate is the anion surfactant of excellent property, present existing more than the 30 kind of popular product in countries in the world, because it has that raw material sources are wide, synthesis technique is simple, production cost is low, new concept and the higher advantages such as surfactivity that skin is gentle, pungency is little, Biosafety is easily degraded, three-waste free pollution etc. met to safety and environmental protection is widely used in the fields such as weaving, printing and dyeing, papermaking, agricultural chemicals, washing, medicine, makeup.Traditional sulphosuccinates permeate agent adopts sulfuric acid to make catalyzer, and the sulfonation transformation efficiency is lower, and osmotic effect is unstable.
The objective of the invention is to solve traditional sulphosuccinates permeate agent sulfonation transformation efficiency lower, the unsettled problem of osmotic effect.Principle of the present invention is on traditional mode of production permeate agent method basis, adopts compound acid as catalyst, by test, finds the impact of all conditions on esterification, determines best processing condition, has reached the stability of product effect.
The technological process of amber acid ester sulfonate permeate agent production can be divided into esterification and sulfonation reaction process.
Esterification reaction process adds MALEIC ANHYDRIDE and the isooctyl alcohol ratio of 1: 3 in molar ratio in reactor, after being heated to the whole fusings of MALEIC ANHYDRIDE, add 0.5% complex acid catalyst, rising temperature to 135 ℃ is reacted, the water generated and band aqua azeotropic, after condensation, water separates through water trap, and the band aqua turns back in reactive system, esterification 3.5h.After end, use the hot wash reaction solution, branch vibration layer, isooctyl alcohol is removed in underpressure distillation, in system, adds in sodium hydroxide and the monoester generated, and the monoester sodium salt can not removed, the direct phase-transfer catalyst as sulfonation reaction.
The sulfonation reaction process: continue to add sodium bisulfite in reactor, distilled water or add in addition phase-transfer catalyst, heat up and reacted, the sulfonated products static layering generated, sulfonated waste water leaches, and adds a certain amount of ethanol, water, has both obtained product sulphosuccinates permeate agent.
The process of preparing of the modified form succinin sulfonate permeate agent the present invention relates to is as follows:
Permeate agent of the present invention is faint yellow to the brown color thick liquid, and solid content is respectively 60%, 70%, and pH is 6.5～7.5, soluble in water, not anti-strong acid, highly basic, heavy metallic salt and reductive agent, infiltration fast, evenly, has good wetting, infiltration, emulsification, lathering property.Former permeate agent is mainly used in, in weaving, dyeing, by the permeate agent after improvement, being introduced into for leatheroid, and it is added in urethane resin, make urethane resin infiltrate fast base cloth (foundation), become long-pending property good, improve stripping strength, the leatheroid abscess is increased, flexible after moulding.
Permeate agent of the present invention has been accelerated speed of response on producing, and has shortened the production time, by original production, within required 14 hours, shortens to 8 hours, has reduced the energy, has reduced cost.
For example:
The present embodiment is implemented take technical solution of the present invention under prerequisite, has provided detailed embodiment and process, can not be interpreted as limiting the scope of the invention.Test method concrete in the following example is as follows.
Step 1, take the 1g sample, puts into volumetric flask, adds water to 1000mL, until sample dissolves fully in water.
Step 2, pour solution in beaker into, the canvas sheet put into to above-mentioned solution and soak, and when the canvas sheet enters solution, starts timing, while sinking to bottom, stops timing, records time t used.
Step 3, repeating step 25 times, record respectively each canvas sheet from entering solution to being sink to bottom time t used
i.
Calculation formula:
Rate of permeation is: [t-(106.4 ÷ 3)+100] * 100%
In formula: t---sample permeates mean time, s;
106.5---canvas sheet radix;
5---number of times;
3---coefficient.
Embodiment 1
Measure at normal temperatures the rate of permeation without the solution that adds permeate agent, acquired results is as following table:
| Temperature ℃ | 25 |
| Solid content % | - |
| Permeate agent quality g | 0 |
| Rate of permeation % | 80.6 |
Embodiment 2
The rate of permeation of the solution of the permeate agent 1.0g that measure to add at normal temperatures solid content be 60%, acquired results is as following table:
| Temperature ℃ | 25 |
| Solid content % | 60 |
| Permeate agent quality g | 1.0 |
| Rate of permeation % | 116 |
Embodiment 3
The rate of permeation of the solution of the permeate agent 1.0g that measure to add at normal temperatures solid content be 70%, acquired results is as following table:
| Temperature ℃ | 25 |
| Solid content % | 70 |
| Permeate agent quality g | 1.0 |
| Rate of permeation % | 135 |
Embodiment 1～3 measures rate of permeation and added and be compared as follows:
| Temperature ℃ | 25 | 25 | 25 |
| Solid content % | - | 60 | 70 |
| Permeate agent quality g | 0 | 1.0 | 1.0 |
| Rate of permeation % | 80.6 | 116 | 135 |
Claims (1)
1. the preparation method of a modified form succinin sulfonate permeate agent, its characterization step is as follows:
(1) esterification:
(2) sulfonation reaction:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101764117A CN103450055A (en) | 2012-05-31 | 2012-05-31 | Preparation method of improved sulfosuccinate penetrant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101764117A CN103450055A (en) | 2012-05-31 | 2012-05-31 | Preparation method of improved sulfosuccinate penetrant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103450055A true CN103450055A (en) | 2013-12-18 |
Family
ID=49732949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101764117A Pending CN103450055A (en) | 2012-05-31 | 2012-05-31 | Preparation method of improved sulfosuccinate penetrant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103450055A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0458099A2 (en) * | 1990-05-25 | 1991-11-27 | Pfersee Chemie GmbH | Process for the preparation of salts of sulfosuccinic acid dialkylesters |
| CN1160710A (en) * | 1996-03-25 | 1997-10-01 | 南京理工大学 | Preparation process of diisooctyl sodium sulfosuccinate |
| CN101284806A (en) * | 2008-06-06 | 2008-10-15 | 江苏省海安石油化工厂 | Clean production process for sodium diethylhexyl sulfosuccinate |
| CN101385954A (en) * | 2007-10-09 | 2009-03-18 | 东南大学 | Preparation method of high pure succinate surfactants for paper manufacturing industry |
| CN102391158A (en) * | 2011-08-04 | 2012-03-28 | 浙江合诚化学有限公司 | Preparation method of isooctanol polyoxypropylene ether sodium sulfosuccinate diester |
-
2012
- 2012-05-31 CN CN2012101764117A patent/CN103450055A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0458099A2 (en) * | 1990-05-25 | 1991-11-27 | Pfersee Chemie GmbH | Process for the preparation of salts of sulfosuccinic acid dialkylesters |
| CN1160710A (en) * | 1996-03-25 | 1997-10-01 | 南京理工大学 | Preparation process of diisooctyl sodium sulfosuccinate |
| CN101385954A (en) * | 2007-10-09 | 2009-03-18 | 东南大学 | Preparation method of high pure succinate surfactants for paper manufacturing industry |
| CN101284806A (en) * | 2008-06-06 | 2008-10-15 | 江苏省海安石油化工厂 | Clean production process for sodium diethylhexyl sulfosuccinate |
| CN102391158A (en) * | 2011-08-04 | 2012-03-28 | 浙江合诚化学有限公司 | Preparation method of isooctanol polyoxypropylene ether sodium sulfosuccinate diester |
Non-Patent Citations (6)
| Title |
|---|
| 张万忠等: "琥珀酸二异辛酯磺酸钠制备的影响因素研究", 《化学试剂》 * |
| 张万忠等: "琥珀酸二异辛酯磺酸钠的合成与新应用", 《材料导报》 * |
| 张跃军等: "快速渗透剂T合成中磺化反应工艺的优化", 《江苏化工》 * |
| 张跃军等: "快速渗透剂T的制备新工艺（Ⅰ）――相转移催化剂的选择", 《南京理工大学学报》 * |
| 成跃祖: "磺基琥珀酸盐的合成改性及应用", 《精细化工》 * |
| 郑延华等: "琥珀酸二烷酯磺酸钠的合成", 《湘潭大学自然科学学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104437645B (en) | Metal-organic framework supported heteropoly acid catalyst for synthesizing glutaraldehyde and production method of metal-organic framework supported heteropoly acid catalyst | |
| CN104264481B (en) | A kind of high temperature alkali resistant bleeding agent and preparation method thereof | |
| CN101830803B (en) | Method for synthesizing citric acid ester type compound | |
| DE2048861A1 (en) | Manufacturing process of Benzvhden sorbitol | |
| CN102391158A (en) | Preparation method of isooctanol polyoxypropylene ether sodium sulfosuccinate diester | |
| CN106631720B (en) | Method for directly synthesizing polymethoxy dimethyl ether by taking dilute formaldehyde and methylal as raw materials | |
| CN102060738A (en) | Ionic liquid combining B acid site and L acid site as well as preparation method and application thereof | |
| CN104492495A (en) | Ionic liquid immobilized magnetic solid acid material catalyst and preparation method thereof | |
| CN102010335A (en) | Method for synthesizing tributyl citrate under catalysis of functional ionic liquid | |
| DE1593200A1 (en) | Process for the production of half-esters | |
| CN106380394A (en) | Preparation method of carbon-silicon solid acid catalyst and application in extraction of organic acid in fermentation broth | |
| CN103450055A (en) | Preparation method of improved sulfosuccinate penetrant | |
| CN102311420A (en) | Method for synthesizing epsilon-caprolactone | |
| CN102659592A (en) | Method for synthesizing tributyl citrate by using resorcinol formaldehyde resin based solid acid as catalyst | |
| CN104529774B (en) | The preparation method of a kind of tributyl citrate | |
| CN102876466B (en) | Method for catalyzing ester exchange reaction with alkaline ionic liquid | |
| CN102786371A (en) | New method for producing alpha,beta-unsaturated carbonyl compounds by using one-pot condensation reaction | |
| CN104667978A (en) | Magnetic core-shell structural solid acid material and preparation method thereof | |
| CN102120796B (en) | Preparation method of fatty alcohol ether modified styrene-maleic anhydride tanning agent | |
| CN103450015A (en) | Synthetic method of tri-n-butyl citrate | |
| CN107519932A (en) | A kind of phase transfer catalyst for benzyl alcohol oxidation synthesizing benzaldehyde and preparation method thereof | |
| CN105294406B (en) | One kind is with solid base CaO/ZrO2The method of catalyst synthesizing polyoxymethylene dimethyl ether | |
| CN105384630B (en) | Hexylene glycol ester of citric acid three and preparation method thereof | |
| CN104230692A (en) | Preparation method of 3,3-dimethyl-1,2-cyclopropane dicarboxylic acid | |
| CN102060737B (en) | Secondary alkyl sodium sulfonate posttreatment method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131218 |