CN102160939A - Self-emulsifying molecular antifoaming agent and preparation method thereof - Google Patents
Self-emulsifying molecular antifoaming agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a self-emulsifying molecular antifoaming agent and a preparation method thereof. The antifoaming agent comprises the following components in percent by mass: 20 to 60 percent of antifoaming active substance and 40 to 80 percent of dispersion medium, wherein the antifoaming active substance consists of higher fatty alcohol, alkynol, polyether and silicone oil in a mass ratio of 1:(0.8-1.5):(2-3):(2-4); and the dispersion medium is grafted star polymer. The preparation method comprises the following steps of: adding 50 to 150 parts of trichloromethane and 1 to 2 parts of p-methyl benzene sulfonic chloride into 20 to 60 mass parts of active substance and 40 to 80 mass parts of star polymer, raising the temperature to between 40 and 70 DEG C, and reacting for 3 to 6 hours; and after the reaction is finished, washing sodium carbonate until the ph is 7, drying by using anhydrous sodium sulfate, and evaporating the solvent under reduced pressure to obtain the antifoaming agent. The extended arm of the star polymer in the antifoaming agent is grafted with the active substance, so that various components are synergistic, and the obtained antifoaming agent is high in stability, low in surface tension, high in surface activity, high in antifoaming capacity, long in foam inhibition time and small in dosage.
Description
Technical field
The present invention relates to defoamer and preparation method thereof, be specifically related to molecular level defoamer of a kind of self-emulsifying that is applied to the star-type polymer type and preparation method thereof.
Background technology
Defoamer is of a great variety on the market, and low-carbon alcohols, mineral oil, polar organic compounds and silicones etc. are arranged.Comparatively speaking, silicone based defoamer is considered in the water-based system defoamer efficiently.A lot of defoamer patents about aqueous based systems are also arranged at present both at home and abroad, and as CN1919936A, US6686320, CN1676544 etc., these are organosilicon or silicon polyethers defoamer, also have mineral oil defoaming agent.Though known defoamer can be good at being utilized to suppressing and eliminates foam in the aqueous based systems, but the requirement that also exists some still can not satisfy or fail to satisfy, so defoamer is with incompatible with water and reach the froth breaking purpose, if handle the bad film coated surface defective that is easy to generate, and stability can not reach satisfied effect, and it can not be taken into account the froth breaking ability, press down bubble ability, wettability, system stability and compatibility etc.
PLA is the material that has biodegradability, biocompatibility concurrently, has obtained using widely at biomedical sector.It has higher intensity and good processing properties, is with a wide range of applications at aspects such as packaging for foodstuff, agricultural, structural timbers as environment-friendly material.Crystal property, hot property, mechanical property and the processing characteristics of hub-and-spoke configuration PLA (s-PLA) is different from the PLA of linear structure.Present research major part is " nuclear " with derivative of the derivative of little molecule polyhydroxy-alcohol, inorganic (heterocycle) compound, metallo-organic compound, polyhydric phenols etc., obtain s-PLA by the lactide ring-opening polymerisation, it is advantageous that molecular weight of product can be by the mole control recently of initator and monomer, but the research that star-like PLA is used for defoamer yet there are no pertinent literature.
Summary of the invention
The objective of the invention is: molecular level defoamer of a kind of self-emulsifying and preparation method thereof is provided, " arm " grafting active material of stretching out by the star-type polymer in the defoamer of the inventive method preparation, make each component Synergistic, defoamer good stability, the surface tension that obtains is little, surface-active is high, the froth breaking ability is strong, press down the bubble time long, consumption is little.
Technical solution of the present invention is: defoamer comprises froth breaking active material and decentralized medium, and the froth breaking active material is the 20-60% of gross mass, and decentralized medium is the 40-80% of gross mass; Wherein, described froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:0.8 ~ 1.5:2 ~ 3:2 ~ 4 is formed by mass ratio, and described decentralized medium is the grafting star-type polymer.
Wherein, the general formula of described higher aliphatic active material is ROH, and R is the long-chain alcohol of C7-C30, is good with C7-C16; Comprising 4-methyl-2-hexanol, isooctanol, 3-enanthol, isomerous tridecanol, the basic decyl alcohol of 2-, tetradecyl alchohol or hexadecanol; Higher aliphatic is the 5-15% of gross mass, is good with 8-15%.
Wherein, the general formula of described alkynol class active material is R
1C ≡ CR
2, R
1And R
2Be identical or different fatty alcohol radicals; It is alkynol or acetylenic glycols, comprises methyl butynol, 2,5-dimethyl-3-hexin-2,5-glycol, 3,5-dimethyl-1-hexin-3-alcohol or 3,6-dimethyl-4-octyne-3,6-glycol; Alkynol class active material is the 5-10% of gross mass, is good with 6-8%.
Wherein, the general structure of described glycerin polyether is R{O (EO)
m(PO)
nH}
3, R is CH
2CH
2CH
2, m and n represent the degree of polymerization of oxirane and expoxy propane, are the integer of 1-50, and molecular weight is 500-2000; Preferred polyoxypropylene glycerin ether or polyoxyethylene polyoxypropylene glycerin ether, glycerin polyether is the 15-25% of gross mass, is good with 15-20%.
Wherein, described silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methyl chloride phenyl silicone oil, methyl ethoxy silicone oil, methyl trifluoro propyl silicone oil, methyl ethylene silicone oil, methyl hydroxy silicon oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil, contains nitrile silicone.
Wherein, the grafting star-type polymer of described decentralized medium is the linear PLA of n arm (ns-PLLA-OH), wherein n=1-6.
Wherein, the preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 50 ~ 150 parts of chloroforms as solvent in 20 ~ 60 parts of active materials and 40 ~ 80 parts of star-type polymers, 1 ~ 2 part of p-methyl benzene sulfonic chloride is warming up to 40 ~ 70 degree as initator, reacts 3 ~ 6 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
The present invention has the following advantages:
1. defoamer of the present invention is composite by star-type polymer, alkynol, higher aliphatic, glycerin polyether and silicone oil, do not need emulsifier, the effect of performance cooperative effect strengthens froth breaking and presses down the bubble ability, makes that the defoamer surface tension is little, the surface-active height, the froth breaking ability is strong, but the bubble time is long, and consumption is little, and the particle diameter of emulsion system has only 200nm, makes defoamer more in a small amount have very strong effect.
2. because adopt star-type polymer,, make that the performance of defoamer is controlled so alkynol, higher aliphatic, glycerin polyether and silicone oil are realized the design of molecular level easily according to how much the arranging in pairs or groups arbitrarily of " arm " of star-type polymer.
3. because be design on the molecular level, make the defoamer chemical property stable, it is above and not stratified to place half a year, is difficult for being gathered into big defoamer drop, avoids disperseing bad and causes adverse consequences.
4. preparation method of the present invention is simple, and processing ease, raw materials for production all can be bought from market and obtain acid-fast alkali-proof, cost performance height.
5. the use of star-like PLA makes this defoamer have biodegradability, biocompatibility, meets environmental protection requirement.
The specific embodiment
Further specify technical scheme of the present invention below by specific embodiment, embodiment can not be interpreted as the restriction to the technology of the present invention solution.
Embodiment 1:
Defoamer comprises froth breaking active material and decentralized medium, the froth breaking active material is 20% of a gross mass, decentralized medium is 80% of a gross mass, the froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:0.8:2:2 is formed by mass ratio, and decentralized medium is the linear PLA of n arm (ns-PLLA-OH) of n=1; Wherein, described higher aliphatic active material is an isooctanol, and described alkynol class active material is 2,5-dimethyl-3-hexin-2 alkynol, and described glycerin polyether is the polyoxypropylene glycerin ether, described silicone oil is methyl-silicone oil.
The preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 50 parts of chloroforms as solvent in 20 parts of active materials and 80 parts of star-type polymers, and 1 part of p-methyl benzene sulfonic chloride is warming up to 40 degree as initator, reacts 3 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
Embodiment 2:
Defoamer comprises froth breaking active material and decentralized medium, the froth breaking active material is 40% of a gross mass, decentralized medium is 60% of a gross mass, the froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:1.1:2.5:3 is formed by mass ratio, and decentralized medium is the linear PLA of n arm (ns-PLLA-OH) of n=3; Wherein, described higher aliphatic active material is the basic decyl alcohol of 2-, and described alkynol class active material is a methyl butynol, and described glycerin polyether is the polyoxyethylene polyoxypropylene glycerin ether, and described silicone oil is methyl trifluoro propyl silicone oil.
The preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 100 parts of chloroforms as solvent in 40 parts of active materials and 60 parts of star-type polymers, and 1.5 parts of p-methyl benzene sulfonic chlorides are warming up to 55 degree as initator, react 4.5 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
Embodiment 3:
Defoamer comprises froth breaking active material and decentralized medium, the froth breaking active material is 60% of a gross mass, decentralized medium is 40% of a gross mass, the froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:1.5:3:4 is formed by mass ratio, and decentralized medium is the linear PLA of n arm (ns-PLLA-OH) of n=6; Wherein, described higher aliphatic active material is 4-methyl-2-hexanol, and described alkynol class active material is 3,5-dimethyl-1-hexin-3-alcohol, and described glycerin polyether is the polyoxyethylene polyoxypropylene glycerin ether, described silicone oil is methyl phenyl silicone oil.
The preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 150 parts of chloroforms as solvent in 60 parts of active materials and 40 parts of star-type polymers, and 2.0 parts of p-methyl benzene sulfonic chlorides are warming up to 70 degree as initator, react 6 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
Embodiment 4:
Defoamer comprises froth breaking active material and decentralized medium, the froth breaking active material is 30% of a gross mass, decentralized medium is 70% of a gross mass, the froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:0.9:2.2:2.5 is formed by mass ratio, and decentralized medium is the linear PLA of n arm (ns-PLLA-OH) of n=2; Wherein, described higher aliphatic active material is the 3-enanthol, and described alkynol class active material is 3,6-dimethyl-4-octyne-3, and 6-glycol, described glycerin polyether are the polyoxypropylene glycerin ether, described silicone oil is methyl ethoxy silicone oil.
The preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 70 parts of chloroforms as solvent in 30 parts of active materials and 70 parts of star-type polymers, and 1.2 parts of p-methyl benzene sulfonic chlorides are warming up to 70 degree as initator, react 6 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
Embodiment 5:
Defoamer comprises froth breaking active material and decentralized medium, the froth breaking active material is 50% of a gross mass, decentralized medium is 50% of a gross mass, the froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:1.3:2.8:3.5 is formed by mass ratio, and decentralized medium is the linear PLA of n arm (ns-PLLA-OH) of n=4; Wherein, described higher aliphatic active material is an isomerous tridecanol, and described alkynol class active material is 3,6-dimethyl-4-octyne-3, and 6-glycol, described glycerin polyether are the polyoxypropylene glycerin ether, described silicone oil is the ethyl containing hydrogen silicone oil.
The preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 120 parts of chloroforms as solvent in 50 parts of active materials and 50 parts of star-type polymers, and 1.8 parts of p-methyl benzene sulfonic chlorides are warming up to 70 degree as initator, react 3 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
Embodiment 6:
Defoamer comprises froth breaking active material and decentralized medium, the froth breaking active material is 35% of a gross mass, decentralized medium is 65% of a gross mass, the froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:1.:3:4 is formed by mass ratio, and decentralized medium is the linear PLA of n arm (ns-PLLA-OH) of n=5; Wherein, described higher aliphatic active material is a hexadecanol, and described alkynol class active material is a methyl butynol, and described glycerin polyether is the polyoxyethylene polyoxypropylene glycerin ether, and described silicone oil is fluorine containing silicone oil.
The preparation method of the molecular level defoamer of self-emulsifying is: mass fraction is to add 100 parts of chloroforms as solvent in what 65 parts of star-type polymer of 35 parts of active materials, and 1.5 parts of p-methyl benzene sulfonic chlorides are warming up to 60 degree as initator, react 5 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
Froth breaking and suds suppressing properties test:
Use the ventilation Bubbling method to measure froth breaking and suds suppressing properties; Take by weighing the sample (being accurate to 0.1mg) of 0.1g, add the dilution of 10ml water and stir evenly, promptly get the defoamer dilution; Taking by weighing 1.0g(and be accurate to 0.1mg) neopelex puts into the 1000ml beaker, adding 400ml water carefully is stirred to molten entirely, beaker is put into thermostat water bath and is incubated, and bubbling instrument bubbling head is positioned over the solution bottom in the beaker again, begins bubbling with 2L/min air-blowing amount, when treating foam to rim of a cup, add the defoamer dilution quickly and evenly, start stopwatch simultaneously, the record foam disappear to the time of liquid level be foam time, foam time is short, and defoaming effect is good; The time that foam is raised to 600ml, 800ml and 1000ml once more is to press down the bubble time, but the bubble time is long more, presses down bubble efficient height; This measurement is at room temperature to carry out, can also be by changing bath temperature with froth breaking and suds suppressing properties under the test different temperatures; The result is as shown in table 1.
Table 1 froth breaking and suds suppressing properties test
Coating that defoamer combines with printing ink and wettability test:
Under the room temperature, 0.1% defoamer is joined in the printing ink of defoamer, take out and to place on a small quantity on the clean glass plate, with spreading rod it is coated with flatly then, observe the state of printing ink on glass plate; The result is as shown in table 2.
Table 2 paintability test result
Claims (10)
1. the molecular level defoamer of self-emulsifying, it is characterized in that: defoamer comprises froth breaking active material and decentralized medium, and the froth breaking active material is the 20-60% of gross mass, and decentralized medium is the 40-80% of gross mass; Wherein, described froth breaking active material is that higher aliphatic, alkynol, polyethers and the silicone oil of 1:0.8 ~ 1.5:2 ~ 3:2 ~ 4 is formed by mass ratio, and described decentralized medium is the grafting star-type polymer.
2. the molecular level defoamer of self-emulsifying according to claim 1, it is characterized in that: the general formula of described higher aliphatic active material is ROH, and R is the long-chain alcohol of C7-C30, and higher aliphatic is the 5-15% of gross mass.
3. the molecular level defoamer of self-emulsifying according to claim 2, it is characterized in that: the general formula of described higher aliphatic active material is ROH, R is the long-chain alcohol of C7-C16, comprise 4-methyl-2-hexanol, isooctanol, 3-enanthol, isomerous tridecanol, the basic decyl alcohol of 2-, tetradecyl alchohol or hexadecanol, higher aliphatic is the 8-15% of gross mass.
4. the molecular level defoamer of self-emulsifying according to claim 1, it is characterized in that: the general formula of described alkynol class active material is R
1C ≡ CR
2, R
1And R
2Be identical or different fatty alcohol radicals, alkynol class active material is the 5-10% of gross mass.
5. the molecular level defoamer of self-emulsifying according to claim 4, it is characterized in that: described alkynol class active material is alkynol or acetylenic glycols, comprise methyl butynol, 2,5-dimethyl-3-hexin-2,5-glycol, 3,5-dimethyl-1-hexin-3-alcohol or 3,6-dimethyl-4-octyne-3, the 6-glycol, alkynol class active material is the 6-8% of gross mass.
6. the molecular level defoamer of self-emulsifying according to claim 1, it is characterized in that: the general structure of described glycerin polyether is R{O (EO)
m(PO)
nH}
3, R is CH
2CH
2CH
2, m and n represent the degree of polymerization of oxirane and expoxy propane, are the integer of 1-50, and molecular weight is 500-2000, and glycerin polyether is the 15-25% of gross mass.
7. the molecular level defoamer of self-emulsifying according to claim 6, it is characterized in that: described glycerin polyether is polyoxypropylene glycerin ether or polyoxyethylene polyoxypropylene glycerin ether, is the 15-20% of gross mass.
8. the molecular level defoamer of self-emulsifying according to claim 1, it is characterized in that: described silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methyl chloride phenyl silicone oil, methyl ethoxy silicone oil, methyl trifluoro propyl silicone oil, methyl ethylene silicone oil, methyl hydroxy silicon oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil, contains nitrile silicone.
9. the molecular level defoamer of self-emulsifying according to claim 1, it is characterized in that: the grafting star-type polymer in the described decentralized medium is the linear PLA of n arm (ns-PLLA-OH), wherein n=1-6.
10. the preparation method of the molecular level defoamer of self-emulsifying according to claim 1, it is characterized in that the preparation method is: mass fraction is to add 50 ~ 150 parts of chloroforms as solvent in 20 ~ 60 parts of active materials and 40 ~ 80 parts of star-type polymers, 1 ~ 2 part of p-methyl benzene sulfonic chloride is as initator, be warming up to 40 ~ 70 degree, reacted 3 ~ 6 hours; Reaction finishes back sodium carbonate and is washed till ph=7, uses anhydrous sodium sulfate drying, and the evaporated under reduced pressure solvent promptly gets defoamer.
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| CN104606926A (en) * | 2015-01-07 | 2015-05-13 | 江苏斯德瑞克化工有限公司 | Silicone-modified vegetable oil polymer polyether defoamer and preparation method thereof |
| CN105031978A (en) * | 2015-08-27 | 2015-11-11 | 杭州彤诚新材料技术有限公司 | Silyl ether mixed defoaming agent emulsion and preparation method thereof |
| CN105561634A (en) * | 2016-01-27 | 2016-05-11 | 西安三业精细化工有限责任公司 | Preparation method of defoaming agent resistant to high temperature and strong alkali |
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