CN107602509A - A kind of beet alkali surface activator and its synthetic method and application - Google Patents
A kind of beet alkali surface activator and its synthetic method and application Download PDFInfo
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- CN107602509A CN107602509A CN201710652622.6A CN201710652622A CN107602509A CN 107602509 A CN107602509 A CN 107602509A CN 201710652622 A CN201710652622 A CN 201710652622A CN 107602509 A CN107602509 A CN 107602509A
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- surface activator
- beet alkali
- alkali surface
- dtpa
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Abstract
The invention discloses a kind of beet alkali surface activator and its synthetic method and application, this method is by diethylene triamine pentacetic acid (DTPA), alkali lye and solvent mix, 70~90 DEG C are warming up to be reacted, obtained solution is rotated, and recrystallized with acetone and ethanol, filtering, dry, obtain diethylene triamine pentacetic acid (DTPA) five sodium-salt, itself and epoxychloropropane and solvent are mixed, pH=9~10 of maintenance system, 60~90 DEG C are warming up to be reacted, obtained solution is rotated, wash and recrystallized with acetone, filtering, dry, obtain beet alkali surface activator.The synthetic method is simple, and reaction condition is gentle, product is easy to purify, and yield is high.The beet alkali surface activator of the present invention has the advantages of wettability is good, foaming abundancy is fine and smooth, bactericidal effect is notable and surface-active is high, can have good compatibility with other types surfactant, can be applied in detergent applications.
Description
Technical field
The invention belongs to technical field of surfactant, more particularly, to a kind of beet alkali surface activator and its conjunction
Into methods and applications.
Background technology
Glycine betaine is the amphoteric surfactant of the atoms of N containing strong basicity, because in its structure simultaneous with anion and sun from
Subbase group, the feature of cation group is presented in an acidic solution, anionic surfactant is presented in alkaline solution
Feature, good surface-active can be kept in the range of wider pH, is widely used in the fields such as food, medicine, chemical industry.
The species of beet alkali ampholytic surface active agent is broadly divided into carboxylic acid type glycine betaine, sulfobetaines, sulfite sweet tea
Dish alkali and phosphate glycine betaine etc., but the synthesis of existing beet alkali surface activator, technically come with some shortcomings.Carboxylic acid
The most frequently used synthetic method of type glycine betaine is that sodium chloroacetate and long-chain alkyl tertiary amine reaction form.Therefore, carried secretly in product not anti-
The amine and sodium chloroacetate answered, make product that there is certain excitant, and the sodium chloride in product is not easy to remove.Sulfobetaines
The production cost of alkali is higher, complex manufacturing and yield are low.Sulfitonetaine is by tertiary amine and the dioxy of stoichiometric proportion
Change the mixture reaction of sulphur and oxirane, but be that sulfur dioxide and oxirane influence in the presence of amine the shortcomings that this method
Under, easily reaction forms polyalkylene sulfite, have impact on the purity of reaction product, it is necessary to special polishing purification means.
The synthetic method of phosphate glycine betaine forms typically by the quaternary ammonium salt of hydroxyl with phosphorylation agent reaction, but the reaction is
Violent exothermic reaction, if reaction temperature control is bad, local temperature is too high so that the carbon in the phosphate of generation on alkyl
Chain aoxidizes and generates alkene, so as to cause product color to deepen.
The content of the invention
A kind of the defects of the invention aims to overcome prior art, there is provided synthesis side of beet alkali surface activator
Method.Carboxyl, epoxy radicals, quaternary ammonium group isoreactivity group are introduced into betaine compound by this method, good so as to assign glycine betaine
Wetting, foaming, decontamination, the performance such as sterilization.This method synthesis is simple, and reaction condition is gentle, product is easy to purify.
The beet alkali surface activator prepared another object of the present invention is to provide a kind of above method.The glycine betaine table
The wettability of face activating agent is good, foaming abundancy is fine and smooth, bactericidal effect is notable and surface-active is high.Lived with other types surface
Property agent has good compatibility.
Still a further object of the present invention is the application for providing above-mentioned beet alkali surface activator.
Above-mentioned purpose of the present invention is achieved by the following technical programs：
A kind of synthetic method of beet alkali surface activator, is comprised the following specific steps that：
S1. neutralization reaction：Diethylene triamine pentacetic acid (DTPA), alkali lye and solvent are mixed, stirring is warming up to 70~90 DEG C of progress
Reaction, obtains solution A；
S2. precision processing process：Solution A is subjected to revolving and removes solvent, and is recrystallized with acetone and ethanol, filtering,
Dry, obtain diethylene triamine pentacetic acid (DTPA) five sodium-salt；
S3. quaterisation：Diethylene triamine pentacetic acid (DTPA) five sodium-salt, epoxychloropropane and solvent obtained by step S2 is mixed
Stirring is closed, pH=9~10 of maintenance system, 60~90 DEG C is warming up to and is reacted, obtain solution B；
S4. precision processing process：Solution B is rotated, removes solvent and unreacted epoxychloropropane, cools down, obtains
Wax-like beet alkali surface activator crude product；
S5. the inorganic salts in wax-like beet alkali surface activator crude product are removed with organic solvent washing, and is carried out with acetone
Recrystallization, filtering, dry, obtain beet alkali surface activator.
Preferably, the alkali lye described in step S1 is that sodium hydrate aqueous solution, aqueous sodium carbonate or sodium acid carbonate are water-soluble
Liquid；The solvent is ethanol, isopropanol or n-butanol, and the mol ratio of alkali is 1 in described diethylene triamine pentacetic acid (DTPA) and alkali lye：
(2.5~6).
Preferably, the time reacted described in step S1 is 0.5~3h.
Preferably, the volume ratio of the acetone described in step S2 and ethanol is 1：(1~2), the temperature of the drying is 25
~80 DEG C, the time of the drying is 8~24h.
Preferably, the mol ratio of the diethylene triamine pentacetic acid (DTPA) five sodium-salt described in step S3 and epoxychloropropane is 1：(3
~4), described solvent is isopropanol, n-butanol or n-amyl alcohol, the solvent and the diethylene triamine pentacetic acid (DTPA) five sodium-salt and
The mass ratio of epoxychloropropane is (0.3~3)：1.
Preferably, the time reacted described in step S3 is 10~18h.
Preferably, the temperature dried described in step S5 is 25~80 DEG C, and the time of the drying is 8~24h.
A kind of beet alkali surface activator is prepared by above-mentioned method.
Shown in the molecular structural formula of the beet alkali surface activator such as formula (1)：
Application of the beet alkali surface activator in detergent applications.
Compared with prior art, the invention has the advantages that：
1. carboxyl, epoxy radicals, quaternary ammonium group isoreactivity group are introduced into betaine compound by the present invention, so as to assign beet
The performances such as the good wetting of alkali, foaming, decontamination, sterilization.This method synthesis is simple, and reaction condition is gentle, product is easy to purify, and produces
Rate is high.
2. the wettability for the beet alkali surface activator that the present invention synthesizes is good, foaming abundancy is fine and smooth, bactericidal effect is notable
And surface-active is high.
3. the beet alkali surface activator that the present invention synthesizes can have good compatibility with other types surfactant.
Brief description of the drawings
Fig. 1 is the synthesis process flow diagram of beet alkali surface activator of the present invention.
Embodiment
Present disclosure is further illustrated with reference to specific embodiment, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagent, method and apparatus.
Fig. 1 is the synthesis process flow diagram of beet alkali surface activator of the present invention.Illustrate beet with reference to embodiment 1-6
The synthesis of alkali surfactant and respective performances.
Embodiment 1
1. the aqueous solution and 30ml ethanol that 11.8g diethylene triamine pentacetic acid (DTPA)s, 6g sodium hydroxides are prepared are added to reaction
In kettle, neutralization reaction is carried out, stirring is warming up to 70 DEG C, after reacting 3h, stops reaction, obtains colourless transparent solution A.
2. above-mentioned solution A is carried out into rotation removes solvent, and is recrystallized with acetone and ethanol, filter, done at 25 DEG C
Dry 24h, obtain product diethylene triamine pentacetic acid (DTPA) five sodium-salt, yield 83.1%.
3. 6.3g diethylene triamine pentacetic acid (DTPA)s five sodium-salt, 4.2g epoxychloropropane and 30ml isopropanols are added to reactor
In, quaterisation, pH=9~10 of maintenance system are carried out, stirring is warming up to 60 DEG C, after reacting 18h, stops reaction, obtains
Clear solution B.
4. above-mentioned solution B is rotated, solvent and unreacted epoxychloropropane are removed, cools down, obtains wax-like beet
Alkali surfactant crude product, washed with ethanol and remove inorganic salts, and recrystallized with acetone, filtered, 24h is dried at 25 DEG C,
Obtain target product beet alkali surface activator, yield 79.2%.
Embodiment 2
1. the aqueous solution and 40ml isopropanols that 11.8g diethylene triamine pentacetic acid (DTPA)s, 8g sodium carbonate are prepared are added to reaction
In kettle, neutralization reaction is carried out, stirring is warming up to 80 DEG C, after reacting 2h, stops reaction, obtains colourless transparent solution A.
2. above-mentioned solution A is carried out into rotation removes solvent, and is recrystallized with acetone and ethanol, filter, done at 60 DEG C
Dry 14h, obtain product diethylene triamine pentacetic acid (DTPA) five sodium-salt, yield 81.5%.
3. 6.3g diethylene triamine pentacetic acid (DTPA)s five sodium-salt, 4.2g epoxychloropropane and 35ml n-butanols are added to reactor
In, quaterisation, pH=9~10 of maintenance system are carried out, stirring is warming up to 80 DEG C, after reacting 14h, stops reaction, obtains
Clear solution B.
4. above-mentioned solution B is rotated, solvent and unreacted epoxychloropropane are removed, cools down, obtains wax-like beet
Alkali surfactant crude product, washed with ethanol and remove inorganic salts, and recrystallized with acetone, filtered, 12h is dried at 60 DEG C,
Obtain target product beet alkali surface activator, yield 78.7%.
Embodiment 3
1. the aqueous solution and 50ml n-butanols that 11.8g diethylene triamine pentacetic acid (DTPA)s, 12.6g sodium acid carbonates are prepared are added to
In reactor, neutralization reaction is carried out, stirring is warming up to 90 DEG C, after reacting 0.5h, stops reaction, obtains colourless transparent solution A.
2. above-mentioned solution A is carried out into revolving removes solvent, and is recrystallized with acetone and ethanol, filter, done at 80 DEG C
Dry 8h, obtain product diethylene triamine pentacetic acid (DTPA) five sodium-salt, yield 83.4%.
3. 6.3g diethylene triamine pentacetic acid (DTPA)s five sodium-salt, 4.2g epoxychloropropane and 25ml n-amyl alcohols are added to reactor
In, quaterisation, pH=9~10 of maintenance system are carried out, stirring is warming up to 90 DEG C, after reacting 10h, stops reaction, obtains
Clear solution B.
4. above-mentioned solution B is rotated, solvent and unreacted epoxychloropropane are removed, cools down, obtains wax-like beet
Alkali surfactant crude product, washed with ethanol and remove inorganic salts, and recrystallized with acetone, filtered, 8h is dried at 80 DEG C, obtain
To target product beet alkali surface activator, yield 80.5%.
Embodiment 4
The beet alkali surface activator that the present invention is synthesized carries out wettability test, is produced by synthesis more of the invention
Wettability of the product under various concentrations, condition of different temperatures, test result are as shown in table 1.
The wettability of the beet alkali surface activator of table 1
Table 1 is the wettability of beet alkali surface activator.As known from Table 1, with beet alkali surface activator concentration
Increase, and the rise of system temperature, the wetability enhancing of beet alkali surface activator, illustrate the glycine betaine table that the present invention synthesizes
Face activating agent has very strong wettability, suitable for detergent compositions.
Embodiment 5
The beet alkali surface activator that synthesizes of the present invention is subjected to bactericidal property test, with minimal inhibitory concentration MIC value and
Minimum bactericidal concentration MBC values weigh the sterilizing ability of product, and its value is smaller, represent that its bactericidal activity is stronger, test result is such as
Shown in table 2.
The bactericidal property of the beet alkali surface activator of table 2
Table 2 is the bactericidal property of beet alkali surface activator.As known from Table 2, the glycine betaine surface-active that the present invention synthesizes
For Escherichia coli, hay bacillus, golden staphylococci and Candida albicans, these four microorganisms have good killing ability for agent,
Bactericidal action especially to Escherichia coli and golden staphylococci is more obvious, therefore the beet alkali surface activator that the present invention synthesizes
Go in sterilizing detergent compositions, play bactericidal and bacteriostatic effect.
Embodiment 6
Foaming properties are determined using mechanical vibration method, the beet alkali surface activator that present invention synthesis obtains is made into 2g/L
The aqueous solution, take the 20mL solution in 100mL with piston graduated cylinder in, 10s high speeds vibrate 20 times, stand 30s postscripts
Foam height is recorded, re-records foam height after 5min, test result is as shown in table 3.
The foaming properties of the beet alkali surface activator of table 3
Table 3 is the foaming properties of beet alkali surface activator.As known from Table 3, the glycine betaine surface-active that the present invention synthesizes
Agent has good foaming properties, suitable for detergent compositions, improves the foaming effect of detergent, improves washability.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine and simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of synthetic method of beet alkali surface activator, it is characterised in that comprise the following specific steps that：
S1. neutralization reaction：Diethylene triamine pentacetic acid (DTPA), alkali lye and solvent are mixed, stirring is warming up to 70~90 DEG C and reacted,
Obtain solution A；
S2. precision processing process：Solution A is subjected to revolving and removes solvent, and is recrystallized with acetone and ethanol, filters, dry,
Obtain diethylene triamine pentacetic acid (DTPA) five sodium-salt；
S3. quaterisation：Diethylene triamine pentacetic acid (DTPA) five sodium-salt obtained by step S2, epoxychloropropane and solvent are mixed and stirred
Mix, pH=9~10 of maintenance system, be warming up to 60~90 DEG C and reacted, obtain solution B；
S4. precision processing process：Solution B is rotated, removes solvent and unreacted epoxychloropropane, cools down, obtains wax-like
Beet alkali surface activator crude product；
S5. the inorganic salts removed in wax-like beet alkali surface activator crude product are washed with ethanol, and are recrystallized with acetone, mistake
Filter, dry, obtain beet alkali surface activator.
2. the synthetic method of beet alkali surface activator according to claim 1, it is characterised in that described in step S1
Alkali lye is sodium hydrate aqueous solution, aqueous sodium carbonate or sodium bicarbonate aqueous solution；The solvent is ethanol, isopropanol or positive fourth
Alcohol, the mol ratio of alkali is 1 in described diethylene triamine pentacetic acid (DTPA) and alkali lye：(2.5~6).
3. the synthetic method of beet alkali surface activator according to claim 1, it is characterised in that anti-described in step S1
The time answered is 0.5~3h.
4. the synthetic method of beet alkali surface activator according to claim 1, it is characterised in that described in step S2
The volume ratio of acetone and ethanol is 1：(1~2), the temperature of the drying is 25~80 DEG C, and the time of the drying is 8~24h.
5. the synthetic method of beet alkali surface activator according to claim 1, it is characterised in that described in step S3
The mol ratio of diethylene triamine pentacetic acid (DTPA) five sodium-salt and epoxychloropropane is 1：(3~4), described solvent are isopropanol, positive fourth
The mass ratio of alcohol or n-amyl alcohol, the solvent and the diethylene triamine pentacetic acid (DTPA) five sodium-salt and epoxychloropropane for (0.3~
3)：1.
6. the synthetic method of beet alkali surface activator according to claim 1, it is characterised in that anti-described in step S3
The time answered is 10~18h.
7. the synthetic method of beet alkali surface activator according to claim 1, it is characterised in that done described in step S5
Dry temperature is 25~80 DEG C, and the time of the drying is 8~24h.
8. a kind of beet alkali surface activator, it is characterised in that the beet alkali surface activator is any by claim 1-7
Method described in is prepared.
9. beet alkali surface activator according to claim 8, it is characterised in that the molecule of the beet alkali surface activator
Shown in structural formula such as formula (1)：
10. application of the beet alkali surface activator of claim 8 or 9 in detergent applications.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108714398A (en) * | 2018-05-03 | 2018-10-30 | 沈阳化工大学 | A kind of poly quaternary surfactant preparation method |
| CN113152090A (en) * | 2021-04-15 | 2021-07-23 | 东华大学 | Antibacterial and antiviral cellulose nanofiber filtering and protecting membrane and preparation method thereof |
| CN113546680A (en) * | 2021-06-30 | 2021-10-26 | 桂林端一技研纳米科技有限责任公司 | Chemical reaction type deodorant containing betaine modified bentonite and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199700A (en) * | 2015-10-13 | 2015-12-30 | 西南石油大学 | Oligomeric betanine type foam drainage agent and preparation method |
| CN106957331A (en) * | 2017-04-17 | 2017-07-18 | 中国石油大学(华东) | A kind of phosphate betaine type polymer-containing sewage in oil field efficient germicide and preparation method thereof |
-
2017
- 2017-08-02 CN CN201710652622.6A patent/CN107602509A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199700A (en) * | 2015-10-13 | 2015-12-30 | 西南石油大学 | Oligomeric betanine type foam drainage agent and preparation method |
| CN106957331A (en) * | 2017-04-17 | 2017-07-18 | 中国石油大学(华东) | A kind of phosphate betaine type polymer-containing sewage in oil field efficient germicide and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108714398A (en) * | 2018-05-03 | 2018-10-30 | 沈阳化工大学 | A kind of poly quaternary surfactant preparation method |
| CN113152090A (en) * | 2021-04-15 | 2021-07-23 | 东华大学 | Antibacterial and antiviral cellulose nanofiber filtering and protecting membrane and preparation method thereof |
| CN113546680A (en) * | 2021-06-30 | 2021-10-26 | 桂林端一技研纳米科技有限责任公司 | Chemical reaction type deodorant containing betaine modified bentonite and preparation method thereof |
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Application publication date: 20180119 |