CN107029630A - A kind of mixed emulsifier - Google Patents
A kind of mixed emulsifier Download PDFInfo
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- CN107029630A CN107029630A CN201710353103.XA CN201710353103A CN107029630A CN 107029630 A CN107029630 A CN 107029630A CN 201710353103 A CN201710353103 A CN 201710353103A CN 107029630 A CN107029630 A CN 107029630A
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- Prior art keywords
- fatty alcohol
- straight chained
- acid
- added
- chained alkyl
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/017—Mixtures of compounds
- C09K23/018—Mixtures of two or more different organic oxygen-containing compounds
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of mixed emulsifier.C23 straight chained alkyl fatty alcohols first are heated to just being completely dissolved by the present invention, add phosphorus esterification reagent, and homogeneous obtains pre-dispersed thing；C23 straight chained alkyls fatty alcohol, antioxidant, chelating agent and catalyst are mixed again, 126 DEG C is warming up to, after C25 straight chained alkyl fatty alcohols are completely dissolved, vacuumize, obtain reactant；Pre-dispersed thing is added in reactant, in reaction under condition of negative pressure；After reaction terminates, 80 DEG C are cooled to, deionized water is added and is hydrolyzed, hydrolysis adds mass percent after terminating and decolourized for 60% H2O2, is incubated；Mass parts Na2HSO3 is added, is incubated；Cooling discharge, obtains high-carbon fatty alcohol phosphate emulsifying agent.Preparation method environmental protection, obtained emulsifier effect is good.
Description
Technical field
The present invention relates to a kind of emulsifying agent, more particularly to a kind of mixed emulsifier.
Background technology
Alkyl phosphate is a kind of anion surface active being made up of phosphate diester, monoesters and non-ionic surface active thing
Agent.Because it has relatively low surface tension and good stability, emulsibility, dispersiveness, wetability, soil release performance and anti-quiet
The performance such as electrical, and its performance is close to natural phosphates, degradable, low irritant, therefore it is widely used in day of weaving
With industries such as chemical industry, cosmetics, food, medicine, agricultural chemicals, synthetic materials.At present, the main collection of domestic fatty alcohol phosphate research
In used in middle low carbon fat alcohol phosphate, the product of exploitation mainly as the surfactant of gentle, low stimulation, such as lauryl
Phosphate（1-isobutyl-3,5-dimethylhexylphosphoric acid）Or laurel alcohol ether phosphate（EO=1,3,9 etc.）, applied to shampoo, shower cream, mildy wash
Deng in product.
In general, high-carbon fatty alcohol phosphate（C≥18）Used mainly as emulsifying agent, in the market high-grade height
Carbon fatty alcohol phosphate emulsifying agent is largely monopolized by offshore company, and price is higher.No matter homemade goodses are from kind, quantity and matter
In amount all with outer state-owned larger gap.High-quality high-carbon fatty alcohol phosphate index be mainly reflected in single dibasic acid esters content,
Free phosphoric acid content, unreacted nonionic thing, color and luster etc..Wherein, monoesters influence emulsibility, water-soluble and antistatic behaviour；It is double
Ester influence is smooth, moistness, therefore single, double ester must have rational collocation, could be balanced in emulsification.In addition, free phosphoric acid, not
The nonionic thing and color and luster of reaction are as far as possible low, do not influence follow-up formula.
The content of the invention
In order to overcome the shortcoming and deficiency of prior art, primary and foremost purpose of the invention is to provide a kind of high-carbon fatty alcohol phosphorus
Acid esters emulsifying agent.Another object of the present invention is to provide described high-carbon fatty alcohol phosphate emulsifying agent.The purpose of the present invention
It is achieved through the following technical solutions：C23 straight chained alkyl fatty alcohols are stirred while heating up；When C23 straight chained alkyl fatty alcohols
Just it is completely dissolved, adds phosphorus esterification reagent, homogeneous obtains pre-dispersed thing, and sealing froth breaking is stand-by；By C23 straight chained alkyls fat
Alcohol, antioxidant, chelating agent and catalyst are mixed, and 126 DEG C, after C23 straight chained alkyl fatty alcohols are completely dissolved, are vacuumized, are obtained
To reactant；Pre-dispersed thing is added in reactant, in reaction under condition of negative pressure；After reaction terminates, 80 DEG C are cooled to, addition is gone
Ionized water is hydrolyzed, and hydrolysis adds mass percent after terminating and decolourized for 60% H2O2, is incubated；Add matter
Measure part Na2HSO3, insulation；Cooling discharge, obtains high-carbon fatty alcohol phosphate emulsifying agent；Wherein, the consumption of each raw material is by as follows
Mass ratio is matched, C23 straight chained alkyl fatty alcohols used：Phosphorus esterification reagent：It is C23 straight chained alkyls fatty alcohol used, anti-
Oxidant, chelating agent, catalyst, H2O2, Na2HSO3 of mass percent 60% are according to 35：18：55：0.02：0.03：0.6：5：
3；Described C23 straight chained alkyl fatty alcohols are at least one of straight chained alkyl fatty alcohol that carbon number is 23；Described C23
Straight chained alkyl fatty alcohol is at least one of C18 fatty alcohols, C20 fatty alcohols and C22 fatty alcohols；Described phosphorus esterification reagent is
At least one of P2O5, orthophosphoric acid, metaphosphoric acid and polyphosphoric acids；Described antioxidant is glutathione, vitamin C, dimension
Raw element E, 2,6 di tert butyl 4 methyl phenol, butylated hydroxy anisole, dibutyl hydroxy toluene, gallic acid and nutgall
At least one of propyl propionate；Described chelating agent is disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, polyacrylic acid
At least one of sodium, etidronic acid and Etidronate disodium；Described catalyst be p-methyl benzenesulfonic acid, paratoluenesulfonic acid sodium salt,
At least one of p-methyl benzenesulfonic acid potassium and paratoluenesulfonic acid ammonium salt；The condition of described homogeneous is：Pressure -0.09~-0.1MPa
Lower homogeneous 5min；The described time vacuumized is 33min；Described adds obtained pre-dispersed thing in obtained reactant
To be operated as follows：In the reactant that 6 additions of obtained pre-dispersed thing point are obtained, per minor tick 22min；Institute
State in the condition reacted under condition of negative pressure be in reacting 9h under -0.09~-0.1MPa condition of negative pressure；Described deionized water
Consumption is equivalent to the 6/10 of described C23 straight chained alkyl fatty alcohol quality；The time of described hydrolysis is 3h；Described insulation
Time be 25min；It is high-carbon fatty alcohol phosphate monoester, high-carbon fatty alcohol phosphate diester, unreacted nonionic thing, free phosphorus
The mixture of acid and water；Wherein, the gross mass percentage of high-carbon fatty alcohol phosphate monoester and high-carbon fatty alcohol phosphate diester is more than
＞ 93%, wherein high-carbon fatty alcohol phosphate monoester content ＞ 82%, the content ＜ 15% of high-carbon fatty alcohol phosphate diester, free phosphorus
Sour and unreacted nonionic thing gross mass percentage ＜ 3%, the content mass percent ＜ 2% of free phosphoric acid, water is surplus；It is excellent
Elect the content 84%, the content 15% of high-carbon fatty alcohol phosphate diester, the content of free phosphoric acid of high-carbon fatty alcohol phosphate monoester as
75%th, unreacted nonionic thing 1%.
The present invention has the following advantages and effect relative to prior art：The emulsifying agent that the present invention is provided is green work
Skill, without using poisonous, hazardous solvent, without " three wastes " discharge, the difference for comparing conventional method is to be pre-dispersed in phosphorus esterification reagent
In the reaction mass of a part, it is to avoid phosphorus esterification reagent locally lumps, the problem of extent of reaction is inadequate.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
By 60 mass parts C18 fatty alcohols（Stearyl alcohol）, 0.05 mass parts butylated hydroxy anisole（BHA）, 0.05 mass parts
EDTA-2Na and 0.5 mass parts p-methyl benzenesulfonic acid are added in reactor A, and stirring is warming up to 110 DEG C, treats that C18 fatty alcohols are completely molten
Xie Hou, vacuumizes 30min；In reactor B, 40 mass parts C18 fatty alcohols are added, stirring is warming up to C18 fatty alcohols and just dissolved
（Temperature is 60 DEG C）, the phosphorylating agent that 20 mass parts are made up of 10 mass parts P2O5 and 10 mass parts orthophosphoric acid is added ,-
Homogeneous 5min is opened under 0.05MPa, pre-dispersed thing is obtained, sealing froth breaking is stand-by；The pre-dispersed thing that will be obtained in reactor B, divides 4
Secondary to be rapidly added in reactor A, per minor tick 15min, after addition is finished, reactor A maintains negative pressure -0.1MPa, continues to react
5h, after question response terminates, is cooled to 75 DEG C.Add 12 mass parts deionized waters to be hydrolyzed, the time is 3h；Hydrolysis terminates
The H2O2 that 3 mass parts concentration are mass percent 30% is added afterwards, 30min is incubated, adds 2.8 mass parts Na2HSO3, is incubated
30min.Cooling discharge, obtains the lily C18 fatty alcohol phosphates emulsifying agent of outward appearance.
The present invention uses the content of mono phosphoric acid ester, dibasic acid esters and free phosphoric acid in potentiometric determination product.Obtained detection
As a result it is as shown in table 1：
Table 1
Index result（Mass percent %）
C18 fatty alcohols phosphate monoester 85.37
C18 fatty alcohols phosphate diester 12.70
Free phosphoric acid 0.46
Unreacted nonionic thing 0.90
Moisture surplus 0.57
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by above-described embodiment
System, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (1)
1. a kind of mixed emulsifier, it is characterised in that comprise the steps of：C23 straight chained alkyl fatty alcohols are stirred while
Heating；When C23 straight chained alkyls fatty alcohol has just been completely dissolved, phosphorus esterification reagent is added, homogeneous obtains pre-dispersed thing, and sealing disappears
Bubble is stand-by；C23 straight chained alkyls fatty alcohol, antioxidant, chelating agent and catalyst are mixed, 126 DEG C, C23 straight chained alkyl fat is treated
After fat alcohol is completely dissolved, vacuumize, obtain reactant；Pre-dispersed thing is added in reactant, in reaction under condition of negative pressure；Reaction
After end, 80 DEG C are cooled to, deionized water is added and is hydrolyzed, hydrolysis adds mass percent after terminating be 60%
H2O2 is decolourized, insulation；Mass parts Na2HSO3 is added, is incubated；Cooling discharge, obtains the emulsification of high-carbon fatty alcohol phosphate
Agent；Wherein, the consumption of each raw material is matched by following mass ratio, C23 straight chained alkyl fatty alcohols used：Phosphorus esterification reagent：
C23 straight chained alkyls fatty alcohol used, antioxidant, chelating agent, catalyst, H2O2, Na2HSO3 of mass percent 60% are pressed
According to 35：18：55：0.02：0.03：0.6：5：3；Described C23 straight chained alkyl fatty alcohols are the straight chained alkyl that carbon number is 23
At least one of fatty alcohol；Described C23 straight chained alkyls fatty alcohol is in C18 fatty alcohols, C20 fatty alcohols and C22 fatty alcohol
At least one；Described phosphorus esterification reagent is at least one of P2O5, orthophosphoric acid, metaphosphoric acid and polyphosphoric acids；Described
Antioxidant is glutathione, vitamin C, vitamin E, 2,6 di tert butyl 4 methyl phenol, butylated hydroxy anisole, two
At least one of butylated hydroxytoluene, gallic acid and propylgallate；Described chelating agent is ethylenediamine tetra-acetic acid two
At least one of sodium, tetrasodium ethylenediamine tetraacetate, Sodium Polyacrylate, etidronic acid and Etidronate disodium；Described catalysis
Agent is at least one of p-methyl benzenesulfonic acid, paratoluenesulfonic acid sodium salt, p-methyl benzenesulfonic acid potassium and paratoluenesulfonic acid ammonium salt；Described homogeneous
Condition be：Homogeneous 5min under pressure -0.09~-0.1MPa；The described time vacuumized is 33min；Described will obtain
Pre-dispersed thing add in obtained reactant to be operated as follows：Obtained pre-dispersed thing is divided 6 times and added
To reactant in, per minor tick 22min；It is described in the condition reacted under condition of negative pressure be in -0.09~-0.1MPa negative pressure
Under the conditions of react 9h；
The consumption of described deionized water is equivalent to the 6/10 of described C23 straight chained alkyl fatty alcohol quality；Described hydrolysis
Time be 3h；The time of described insulation is 25min；It is high-carbon fatty alcohol phosphate monoester, high-carbon fatty alcohol phosphate diester, not
The mixture of the nonionic thing of reaction, free phosphoric acid and water；Wherein, high-carbon fatty alcohol phosphate monoester and high-carbon fatty alcohol phosphoric acid are double
The gross mass percentage of ester is more than ＞ 93%, and the wherein content ＞ 82% of high-carbon fatty alcohol phosphate monoester, high-carbon fatty alcohol phosphoric acid are double
The content ＜ 15% of ester, free phosphoric acid and unreacted nonionic thing gross mass percentage ＜ 3%, the content quality hundred of free phosphoric acid
Divide than ＜ 2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710353103.XA CN107029630A (en) | 2017-05-18 | 2017-05-18 | A kind of mixed emulsifier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710353103.XA CN107029630A (en) | 2017-05-18 | 2017-05-18 | A kind of mixed emulsifier |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107029630A true CN107029630A (en) | 2017-08-11 |
Family
ID=59538616
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710353103.XA Withdrawn CN107029630A (en) | 2017-05-18 | 2017-05-18 | A kind of mixed emulsifier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107029630A (en) |
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2017
- 2017-05-18 CN CN201710353103.XA patent/CN107029630A/en not_active Withdrawn
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Application publication date: 20170811 |
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