CN102940982A - High-efficiency defoaming agent for biological fermentation system and preparation process of high-efficiency defoaming agent - Google Patents
High-efficiency defoaming agent for biological fermentation system and preparation process of high-efficiency defoaming agent Download PDFInfo
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Abstract
The invention relates to a high-efficiency defoaming agent for a biological fermentation system and a preparation process of the high-efficiency defoaming agent. The high-efficiency defoaming agent comprises 15-25 parts of organopolysiloxane, 0.5-3 parts of hydrophobic gaseous phase white carbon black, 5-15 parts of polyether modified silicone oil, 0.2-2 parts of silicon resin, 4-10 parts of a food-grade emulsifier, 0.2-2 parts of a food-grade dispersing thickening agent, 0.2-2 parts of a sodium hydroxide solution with the mass concentration of 10% and 40-80 parts of deionized water. The preparation process of the defoaming agent comprises that the organopolysiloxane, the hydrophobic gaseous phase white carbon black and the silicon resin are subjected to high-temperature bonding. If the viscosity of the organopolysiloxane is lower than 20000CST, a method for adding the emulsifier in an aqueous phase can be used, a method for adding the emulsifier in an oil phase can also be used, and if the viscosity of the organopolysiloxane is higher than 20000CST, the method for adding the emulsifier in an oil phase can be used for preparing the defoaming agent. The defoaming agent is fast in defoaming speed and high in foam inhibition ability. The defoaming agent is particularly excellent in terms of defoaming and foam inhibition effects in the microbial fermentation system, and no side effect is produced for production.
Description
Technical field
The present invention relates to a kind of defoamer, particularly a kind of high effective antifoaming agent for the biofermentation system and preparation method thereof.Belong to chemical technology field.
Background technology
The microbial fermentation system is a typical aqueous based systems, during the fermentation, promotes thalli growth owing to will replenish a large amount of aseptic fresh airs, and wind supply quantity increases, and therefore can produce a large amount of foams, and fermentation tank also usually is full of by foam.The existence of a large amount of foams not only can make the actual volume available in the fermentation tank greatly reduce, and causes nutrient solution to overflow from fermentation tank, and can affect the metabolic processes of microorganism, and make product inhomogeneous.Therefore, it is very important to eliminate the harm of these foams.Suppressing these foams method commonly used is to add polyether antifoam agent or silicone defoaming agent, but independent use polyether antifoam agent or organosilyl defoamer often can not have simultaneously instant froth breaking concurrently and press down bubble persistence double properties.Therefore rear the sale mixed with silicone defoaming agent and polyether antifoam agent by the producer that has, in the hope of obtaining preferably resultant effect, but only two kinds of defoamers are simply mixed, not only combination property is still not ideal enough, and this defoamer stability often has problems, the generation of the phenomenon such as layering can be caused, different period antifoam content and the inhomogeneous situation of performance can be caused during interpolation.
Summary of the invention
The objective of the invention is: have good defoaming effect concurrently and press down persistent high effective antifoaming agent for the biofermentation system of bubble and preparation method thereof for the microbial fermentation system provides a kind of, it has solved in the sweat owing to ventilation, stir the practical volume minimizing of the fermentation tank that causes, foam overflow, the inhomogeneous problem of product quality.High effective antifoaming agent of the present invention has good antifoaming performance, is a kind of efficient aqueous based systems defoamer.
The present invention realizes by the following technical solutions: a kind of high effective antifoaming agent for the biofermentation system is characterized in that it is comprised of by following mass parts following component: organopolysiloxane is that 15-25 part, hydrophobic gas-phase silica are that 0.5-3 part, polyether modified silicon oil are that 5-15 part, silicones are that 0.2-2 part, food grade emulsifier are that 4-10 part, food-grade dispersion thickener are that 0.2-2 part, mass concentration are that 10% sodium hydroxide solution is that 0.2-2 part and deionized water are 40-80 part.
Described organopolysiloxane, what link to each other with silicon atom on its silica chain can be various forms of alkyl or hydroxyl, generally selecting the alkyl that links to each other with silicon atom is methyl, and selects the dimethicone of trimethyl end-blocking or hydroxy-end capped dimethicone.
Described hydrophobic gas-phase silica is the hydrophily white carbon through hydrophobic treatments.
Described silicones is MQ type silicones.
Described food grade emulsifier comprises non-ionic surface active agent, anion surfactant, and its HLB value is selected 7.0-10.5.
Described food-grade disperses thickener to disperse thickener for natural food-grade, also can be that the food-grade of synthesizing is disperseed thickener.
A kind of high effective antifoaming agent for the biofermentation system, its preparation method comprises the following steps:
1) take by weighing raw material by following mass parts:
Getting organopolysiloxane is that 15-25 part, hydrophobic gas-phase silica are that 0.5-3 part, polyether modified silicon oil are that 5-15 part, silicones are that 0.2-2 part, food grade emulsifier are that 4-10 part, food-grade dispersion thickener are that 0.2-2 part, mass concentration are that 10% sodium hydroxide solution is that 0.2-2 part and deionized water are 40-80 part;
2) organopolysiloxane of above-mentioned mass parts, hydrophobic gas-phase silica and silicones are added in the electrical heating tank, be warming up under 180-240 ℃, keep and stirred 1-3 hour, namely get silicon cream;
3) high effective antifoaming agent for the preparation of the biofermentation system both can adopt emulsifying agent to add the water method, also can adopt emulsifying agent to add the oil phase method; Organopolysiloxane viscosity both can adopt emulsifying agent to be added in the water method below 20000CST, also can adopt emulsifying agent to be added in the oil phase method, and organopolysiloxane viscosity then adopts emulsifying agent adding oil phase legal system standby more than 20000CST;
Adopt emulsifying agent to add the water method:
3-1) disperse thickener to melt 50-60 ℃ of lower the stirring deionized water of above-mentioned mass parts and the food-grade of above-mentioned mass parts, the mass concentration that adds above-mentioned mass parts is 10% sodium hydroxide solution temperature rise to 75 ℃, adds the mixing of food grade emulsifier of above-mentioned mass parts;
3-2) the silicon cream of step 2 and the polyether modified silicon oil of above-mentioned mass parts are joined step 3-1) stirred 1-3 hour in 75 ℃ of lower emulsifications of temperature in the mixture, get emulsion;
3-3) emulsion is carried out high shear homogeneous or colloid mill homogeneous 0.5-1.5 hour being lower than under 55 ℃ of temperature, get finished product;
Adopt emulsifying agent to add the oil phase method:
3-a) polyether modified silicon oil and the food grade emulsifier with step 2 silicon cream, above-mentioned mass parts mixes 1-3 hour under 75 ℃ of temperature;
3-b) will account in the mixture that above-mentioned mass parts 1/3-1/2 deionized water adds step 3-a and stir 1-3 hour 75 ℃ of emulsifications, get emulsion;
3-c) emulsion was carried out high shear homogeneous or colloid mill homogeneous 0.5-1.5 hour being lower than under 55 ℃ of temperature, make emulsion particle diameter be in 2-30um;
3-d) disperse thickener to be dissolved in remaining deionized water for stirring under 50-60 ℃ the food-grade of above-mentioned mass parts and melt, the mass concentration that adds above-mentioned mass parts is that 10% NaOH stirs, and gets viscous water;
3-e) viscous water is slowly added in the emulsion of step 3-c under stirring, keep and stirred 20-30 minute, until mix; Get finished product.
Described non-ionic surface active agent is this dish, tween, brij72 emulsifying agent or brij721 emulsifying agent; Anion surfactant is lauryl sodium sulfate; The HLB value is selected 7.0-10.5.
It is sodium alginate that described natural food-grade is disperseed thickener, and it is such as xanthan gum or carboxymethyl cellulose that synthetic food-grade is disperseed thickener.
The preparation method of described polyether modified silicon oil is: with the containing hydrogen silicone oil of hydrogeneous matrix amount percentage 0.2-2.0%, containing hydrogen silicone oil accounts for the mass percent 30% of reaction raw materials and the polyethers of the double bond containing polyoxyethylene of end group, polyoxypropylene block polymerization, polyethers accounts for the mass percent 70% of reaction raw materials, above-mentioned raw materials is added in the flask, be warming up to 60 degree, the platinum chloric acid or the trifluoroacetic acid that add the quality 100ppm that accounts for reaction raw materials carry out catalysis, then under 100-120 degree temperature, through hydrosilylation, 4-5 hour and make;
Described polyether modified silicon oil also can directly be bought, the key technical indexes: the light yellow transparent oily liquid of outward appearance; Temperature is in the time of 25 ℃, and density is 1.03 g/cm
3Viscosity is 1500 ~ 4000CS; Cloud point is 47 ℃; Effective ingredient 〉=99.5%.
The invention has the beneficial effects as follows: technology of the present invention compared with prior art, this high effective antifoaming agent for the biofermentation system of the present invention, design on upper and the preparation method from the composition of active material, all taken into full account the rapidity of its froth breaking, the persistence that presses down bubble and the aspects factors such as stability of emulsion.And make each factor obtain splendid combination.The prepared defoamer of the present invention has good effect in most of water-based systems.Especially in the microbial fermentation system, not only can eliminate rapidly owing to ventilate, stir the foam that causes, the also again generation of sustainable inhibition system foam in whole production process.Froth breaking, to press down the bubble effect all very excellent.
The specific embodiment
Below by the specific embodiment that provides the present invention is described clearly further, but not as a limitation of the invention.
Embodiment 1
A kind of high effective antifoaming agent for the biofermentation system, its preparation method comprises the following steps:
1) take by weighing raw material by following mass parts:
Getting organopolysiloxane is that 15kg, hydrophobic gas-phase silica are that 0.5 kg, polyether modified silicon oil are that 5 kg, silicones are that 0.2 kg, food grade emulsifier are that 4 kg, food-grade dispersion thickener are that 0.2 kg, mass concentration are that 10% sodium hydroxide solution is that 0.2 kg and deionized water are 40 kg;
2) organopolysiloxane of 15kg, hydrophobic gas-phase silica and 0.2 silicones of 0.5 kg are added in the electrical heating tank, be warming up under 180-240 ℃, keep and stirred 1-3 hour, namely get silicon cream;
3) organopolysiloxane viscosity adopts emulsifying agent to be added in the water method below 20000CST, also can adopt emulsifying agent to be added in the oil phase method,
Present embodiment adopts emulsifying agent to add the water method:
3-1) 40 kg deionized waters and 0.2 kg food-grade are disperseed thickener melt 50-60 ℃ of lower the stirring, the mass concentration that adds 0.2 kg is 10% sodium hydroxide solution temperature rise to 75 ℃, adds the mixing of food grade emulsifier of 4 kg;
3-2) the silicon cream of step 2 and the polyether modified silicon oil of 5 kg are joined step 3-1) stirred 1-3 hour in 75 ℃ of lower emulsifications of temperature in the mixture, get emulsion;
3-3) emulsion is carried out high shear homogeneous or colloid mill homogeneous 0.5-1.5 hour being lower than under 55 ℃ of temperature, get finished product;
Described organopolysiloxane, what link to each other with silicon atom on its silica chain is various forms of alkyl or hydroxyl, selects the dimethicone of trimethyl end-blocking or hydroxy-end capped dimethicone.Described hydrophobic gas-phase silica is the hydrophily white carbon through hydrophobic treatments.During hydrophobic treatments, water-repelling agent is selected HDMS, DMC class material, selects the white carbon specific area at 150-300M
2/ g.
Described silicones is MQ type silicones.MQ type silicones is the extraordinary silicones of a class that is made of four degree of functionality siloxanes polycondensation chain links and single functionality siloxanes sealing chain link.The molal weight of MQ type silicones is generally 1000 ~ 8000g/mol.The mole of the M chain link in the molecular structure is the properties and applications scope of the structures shape resin of M chain link when.Selecting the ratio of n (M)/n (Q) in the MQ silicones is 0.1-1.0.
It is sodium alginate that described food-grade is disperseed thickener; Described food grade emulsifier is this dish, and it belongs to non-ionic surface active agent.
The preparation method of described polyether modified silicon oil is: be the containing hydrogen silicone oil of 0.2-2.0% with hydrogeneous matrix amount percentage, containing hydrogen silicone oil accounts for the mass percent 30% of reaction raw materials and the polyethers of the double bond containing polyoxyethylene of end group, polyoxypropylene block polymerization, polyethers accounts for the mass percent 70% of reaction raw materials and reacts, method is that above-mentioned raw materials is added in the flask, be warming up to 60 degree, the platinum chloric acid or the trifluoroacetic acid that add the quality 100ppm that accounts for reaction raw materials carry out catalysis, then under 100-120 degree temperature, through hydrosilylation, 4-5 hour and make.
Embodiment 2
Basic identical with embodiment 1, difference is: organopolysiloxane is that 25kg, hydrophobic gas-phase silica are that 3kg, polyether modified silicon oil are that 15kg, silicones are that 2kg, food grade emulsifier are that 10kg, food-grade dispersion thickener are that 2kg, mass concentration are that 10% sodium hydroxide solution is that 2kg and deionized water are 80kg.It is xanthan gum that described food-grade is disperseed thickener; Described food grade emulsifier is tween, and it belongs to non-ionic surface active agent.
Described polyether modified silicon oil is available from the industrial organosilicon new material in Qingdao Co., Ltd, address: economic development zone, Laixi, Qingdao City Zhujiang River road phone 86-0532-88431918.Described polyether modified silicon oil the key technical indexes: the light yellow transparent oily liquid of outward appearance; Temperature is in the time of 25 ℃, and density is 1.03 g/cm
3Viscosity is 1500 ~ 4000CS; Cloud point is 47 ℃; Effective ingredient 〉=99.5%.
Embodiment 3
Basic identical with embodiment 1, difference is: organopolysiloxane is that 20kg, hydrophobic gas-phase silica are that 1.5kg, polyether modified silicon oil are that 10kg, silicones are that 1kg, food grade emulsifier are that 8kg, food-grade dispersion thickener are that 1kg, mass concentration are that 10% sodium hydroxide solution is that 1.2kg and deionized water are 50kg.It is carboxymethyl cellulose that described food-grade is disperseed thickener; Described food grade emulsifier is lauryl sodium sulfate, and it belongs to anion surfactant.
Described organopolysiloxane viscosity then adopts emulsifying agent adding oil phase legal system standby more than 20000CST:
3-a) polyether modified silicon oil and the 8kg food grade emulsifier with step 2 silicon cream, 10kg mixes 1-3 hour under 75 ℃ of temperature;
3-b) stirred 1-3 hour 75 ℃ of emulsifications in the mixture with 25kg deionized water adding step 3-a, get emulsion; The consumption of deionized water: removing ionized water total amount 1/3-1/2 can;
3-c) emulsion was carried out high shear homogeneous or colloid mill homogeneous 0.5-1.5 hour being lower than under 55 ℃ of temperature, make emulsion particle diameter be in 2-30um;
3-d) disperse thickener to be dissolved in remaining 25kg deionized water for stirring under 50-60 ℃ the 1kg food-grade and melt, the mass concentration that adds 1.2kg is that 10% NaOH stirs, and gets viscous water;
3-e) viscous water is slowly added in the emulsion of step 3-c under stirring, keep and stirred 20-30 minute, until mix; Get finished product.
Embodiment 4
1, takes by weighing raw material by following prescription: get 1000CST dimethyl silicone polymer 232.5KG;
Getting specific area is 200M
2The hydrophobic gas-phase silica 12.5KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 5KG; Get polyether modified silicon oil 80KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 33.8KG of span60; Tween60 is 16.2KG altogether; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 619.1KG.
2, the preparation method of this defoamer comprises the following steps: (this example adopts emulsifying agent to be added in the water method)
1) preparation of silicon cream: the dimethyl silicone polymer of above-mentioned mass parts, hydrophobic gas-phase silica, MQ silicones are added in the electrical heating tank, be warming up to 200 ℃, keep and stirred 2-3 hour, make silicon cream.(but MQ silicones also equitemperature is down to adding about 140-150 ℃, and the silicon cream color and luster that makes like this is better).
2) deionized water of above-mentioned mass parts, food thickening agent RHODICARE H are added in the still melt 50-60 ℃ of lower the stirring.Add 10% sodium hydroxide solution, with still temperature rise to 75 ℃, add emulsifying agent span60 and the tween60 of above-mentioned mass parts, stir.Add again the silicon cream of step 1) preparation, carried out fully emulsified 1-3 hour.
3) with step 2) emulsion of preparation imports high shear homogeneous still homogeneous 15-20 minute.Then check, weigh, pack, make defoamer of the present invention.
Embodiment 5
1, takes by weighing raw material by following prescription: get 5000CST dimethyl silicone polymer 232.5KG;
Getting specific area is 200M
2The hydrophobic gas-phase silica 10KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 7.5KG; Get polyether modified silicon oil 90KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 33.8KG of span60; Tween60 is 16.2KG altogether; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 607.9KG.
2, the preparation method adopts emulsifying agent to be added in the water method with embodiment 4(present embodiment).
Embodiment 6
1, takes by weighing raw material by following prescription: get 10000CST dimethyl silicone polymer 211.6KG;
Getting specific area is 200M
2The hydrophobic gas-phase silica 11.5KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 6.9KG; Get polyether modified silicon oil 90KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 40.6KG of span60; Tween60 is 19.4KG altogether; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 617.9KG.
2, the preparation method adopts emulsifying agent to be added in the water method with embodiment 4(present embodiment).
Embodiment 7
1, takes by weighing raw material by following prescription: get 30000CST dimethyl silicone polymer 180.4KG; Get 500CST dimethyl silicone polymer 22KG; Getting specific area is 200M
2The hydrophobic gas-phase silica 13.2KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 4.4KG; Get polyether modified silicon oil 100KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 41.7KG of span60; Get altogether 18.3KG of Brij721; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 617.9KG.
2, the preparation method of this defoamer comprises the following steps: (this example adopts emulsifying agent to be added in the oil phase method)
1) preparation of silicon cream: the dimethyl silicone polymer of above-mentioned mass parts, hydrophobic gas-phase silica, MQ silicones are added in the electrical heating tank, be warming up to 220 ℃, keep and stirred 2-3 hour, make silicon cream.(but MQ silicones also equitemperature is down to adding about 140-150 ℃, and the silicon cream color and luster that makes like this is better).
2) with the silicon cream of step 1) preparation and emulsifying agent, the polyether modified silicon oil of above-mentioned mass parts
Add reactor, be warming up to 75 ℃ and carried out stirring and emulsifying 1-3 hour.Then slowly add emulsified water (emulsified water accounts for 30 parts of defoamer mass parts), emulsification was stirred 1-2 hour.Be cooled to about 55 ℃, cross the colloid mill homogeneous, make emulsion particle diameter be in 2-30um.
3) preparing in advance viscous water (is dissolved in the food thickening agent of above-mentioned mass parts in the residue water 50-60 ℃ the time, the 10% NaOH emulsion that adds above-mentioned mass parts, stir), and viscous water slowly added in the emulsion of colloid mill homogeneous under the stirring, keep and stirred 20-30 minute, until mix.Then check, weigh, pack, make defoamer of the present invention.
Embodiment 8
1, takes by weighing raw material by following prescription: get 50000CST dimethyl silicone polymer 160KG; Get 1000CST dimethyl silicone polymer 24KG; Getting specific area is 200M
2The hydrophobic gas-phase silica 10KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 6KG; Get polyether modified silicon oil 100KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 45.1KG of span60; Get altogether 19.9KG of Brij721; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 632.9KG.
2, the preparation method adopts emulsifying agent to be added in the oil phase method with this example of embodiment 7().
Embodiment 9
1, takes by weighing raw material by following prescription: get 60000CST dimethyl silicone polymer 150KG; Get 350CST dimethyl silicone polymer 34KG; Getting specific area is 200M
2The hydrophobic gas-phase silica 11KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 5KG; Get polyether modified silicon oil 110KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 46KG of Brij72; Get altogether 19KG of Brij721; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 622.9KG.
2, the preparation method adopts emulsifying agent to be added in the oil phase method with this example of embodiment 7().
Embodiment 10
1, takes by weighing raw material by following prescription: get 100000CST dimethyl silicone polymer 126KG; Get 500CST dimethyl silicone polymer 39.6KG; Getting specific area is 200M
2The hydrophobic gas-phase silica 9KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 5.4KG; Get polyether modified silicon oil 120KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 48.6KG of span60; Get altogether 21.4KG of Brij721; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 627.9KG.
2, the preparation method adopts emulsifying agent to be added in the oil phase method with this example of embodiment 7().
Embodiment 11
1, takes by weighing raw material by following prescription: get 100000CST dimethyl silicone polymer 126KG; Get 1000CST dimethyl silicone polymer 39.6KG; Getting specific area is 200M
2The hydrophobic gas-phase silica 9KG of/g; The ratio of getting n (M)/n (Q) is 0.8 silicones 5.4KG; Get polyether modified silicon oil 120KG (polyether modified silicon oil can make in advance by the method for introducing in the aforementioned summary of the invention, also can choose in market the polyether modified silicon oil commodity that meet the demands); Get altogether 49.5KG of Brij72; Get altogether 20.5KG of Brij721; Get RHODICARE H food thickening agent 0.8KG; Get 10% NaOH 1.3KG; Remove ionized water 627.9KG.
2, the preparation method adopts emulsifying agent to be added in the oil phase method with this example of embodiment 7().
Raw materials market in above-described embodiment is all on sale, wherein:
The dimethyl silicone polymer of all size (dimethicone) Dow corning company produces, and NCM sells;
Emulsifying agent span60(Si dish), emulsifying agent tween60 (tween): Jiangsu Hai'an Petrochemical Plant produces, this factory factory site: No. 28, seaization road, county town, Hai'an, Jiangsu Province, postcode: 226600;
Hydrophobic gas-phase silica: Shenyang Chemical Manufacture;
The MQ silicones: Shandong Dayi Chemical Industry Co., Ltd produces;
RHODICARE H(xanthan gum) food thickening agent: French sieve ground is inferior to be produced, and Guangzhou alizarin chemical industry in morning Co., Ltd sells;
Emulsifying agent Brij72 [polyoxyethylene (2) stearyl ether], Brij721[polyoxyethylene (21) stearyl ether]: Kening Co.,Ltd produces, and Guangzhou is prayed the company of liter and sold.
Effect assessment test of the present invention and result
Foaming system: with (80-90 ℃ was kept 30 minutes) under the high temperature 10% dregs of beans filtrate is as foaming system.
Defoamer: the finished product that adopts embodiment 1-11.
Froth breaking, press down the bubble effect evaluation method: in the 500ml graduated cylinder, add the 100ml expanding foam solution, then with the air-blowing head of 50L/h speed by being covered with micropore from graduated cylinder bottom air-blowing, when foam reaches 500ml, to wherein adding the 0.01g defoamer, observe its defoaming effect; After ventilation 10 minutes, measure the amount of foam, as the evaluation foundation of suds suppressing properties.
| Embodiment | Defoaming effect | But the bubble effect (foam volume, ml) |
| Blank | Froth breaking not | 755 |
| GPE | 80s | 420 |
| 1 | 58s | 310 |
| 2 | 43s | 285 |
| 3 | 51s | 299 |
| 4 | 48s | 295 |
| 5 | 31s | 270 |
| 6 | 25s | 250 |
| 7 | 19s | 230 |
| 8 | 16s | 210 |
| 9 | 13s | 210 |
| 10 | 9s | 200 |
| 11 | 7s | 200 |
Find out that from upper table embodiment 1-embodiment 11 all has good froth breaking, presses down the bubble effect, and along with the increase of polysiloxane molecule amount, its froth breaking, press down the bubble better effects if.
Claims (10)
1. high effective antifoaming agent that is used for the biofermentation system is characterized in that it is comprised of by following mass parts following component: organopolysiloxane is that 15-25 part, hydrophobic gas-phase silica are that 0.5-3 part, polyether modified silicon oil are that 5-15 part, silicones are that 0.2-2 part, food grade emulsifier are that to disperse thickener be that 0.2-2 part, mass concentration are that 10% sodium hydroxide solution is that 0.2-2 part and deionized water are 40-80 part for 4-10 part, food-grade.
2. a kind of high effective antifoaming agent for the biofermentation system according to claim 1, it is characterized in that: described organopolysiloxane, what link to each other with silicon atom on its silica chain can be various forms of alkyl or hydroxyl, generally selecting the alkyl that links to each other with silicon atom is methyl, and selects the dimethicone of trimethyl end-blocking or hydroxy-end capped dimethicone.
3. a kind of high effective antifoaming agent for the biofermentation system according to claim 1, it is characterized in that: described hydrophobic gas-phase silica is the hydrophily white carbon through hydrophobic treatments.
4. a kind of high effective antifoaming agent for the biofermentation system according to claim 1, it is characterized in that: described silicones is MQ type silicones.
5. a kind of high effective antifoaming agent for the biofermentation system according to claim 1, it is characterized in that: described food grade emulsifier comprises non-ionic surface active agent, anion surfactant, its HLB value is selected 7.0-10.5.
6. a kind of biofermentation system high effective antifoaming agent according to claim 1 is characterized in that: it can be that natural food-grade is disperseed thickener that described food-grade is disperseed thickener, also can be that the food-grade of synthesizing is disperseed thickener.
7. high effective antifoaming agent that is used for the biofermentation system, its preparation method comprises the following steps:
1) take by weighing raw material by following mass parts:
Getting organopolysiloxane is that 15-25 part, hydrophobic gas-phase silica are that 0.5-3 part, polyether modified silicon oil are that 5-15 part, silicones are that 0.2-2 part, food grade emulsifier are that 4-10 part, food-grade dispersion thickener are that 0.2-2 part, mass concentration are that 10% sodium hydroxide solution is that 0.2-2 part and deionized water are 40-80 part;
2) organopolysiloxane of above-mentioned mass parts, hydrophobic gas-phase silica and silicones are added in the electrical heating tank, be warming up under 180-240 ℃, keep and stirred 1-3 hour, namely get silicon cream;
3) high effective antifoaming agent for the preparation of the biofermentation system both can adopt emulsifying agent to add the water method, also can adopt emulsifying agent to add the oil phase method; Organopolysiloxane viscosity both can adopt emulsifying agent to be added in the water method below 20000CST, also can adopt emulsifying agent to be added in the oil phase method, and organopolysiloxane viscosity then adopts emulsifying agent adding oil phase legal system standby more than 20000CST;
Adopt emulsifying agent to add the water method:
3-1) disperse thickener to melt 50-60 ℃ of lower the stirring deionized water of above-mentioned mass parts and the food-grade of above-mentioned mass parts, the mass concentration that adds above-mentioned mass parts is 10% sodium hydroxide solution temperature rise to 75 ℃, adds the mixing of food grade emulsifier of above-mentioned mass parts;
3-2) the silicon cream of step 2 and the polyether modified silicon oil of above-mentioned mass parts are joined step 3-1) stirred 1-3 hour in 75 ℃ of lower emulsifications of temperature in the mixture, get emulsion;
3-3) emulsion is carried out high shear homogeneous or colloid mill homogeneous 0.5-1.5 hour being lower than under 55 ℃ of temperature, get finished product;
Adopt emulsifying agent to add the oil phase method:
3-a) polyether modified silicon oil and the food grade emulsifier with step 2 silicon cream, above-mentioned mass parts mixes 1-3 hour under 75 ℃ of temperature;
3-b) will account in the mixture that above-mentioned mass parts 1/3-1/2 deionized water adds step 3-a and stir 1-3 hour 75 ℃ of emulsifications, get emulsion;
3-c) emulsion was carried out high shear homogeneous or colloid mill homogeneous 0.5-1.5 hour being lower than under 55 ℃ of temperature, make emulsion particle diameter be in 2-30um;
3-d) disperse thickener to be dissolved in remaining deionized water for stirring under 50-60 ℃ the food-grade of above-mentioned mass parts and melt, the mass concentration that adds above-mentioned mass parts is that 10% NaOH stirs, and gets viscous water;
3-e) viscous water is slowly added in the emulsion of step 3-c under stirring, keep and stirred 20-30 minute, until mix; Get finished product.
8. a kind of high effective antifoaming agent for the biofermentation system according to claim 5 is characterized in that: described non-ionic surface active agent is this dish, tween, brij72 emulsifying agent or brij721 emulsifying agent; Anion surfactant is lauryl sodium sulfate; The HLB value is selected 7.0-10.5.
9. a kind of biofermentation system high effective antifoaming agent according to claim 6 is characterized in that: it is sodium alginate that described natural food-grade is disperseed thickener, and it is xanthan gum or carboxymethyl cellulose that synthetic food-grade is disperseed thickener.
10. according to claim 1 or 7 described a kind of biofermentation system high effective antifoaming agents, it is characterized in that: the preparation method of described polyether modified silicon oil is: be the containing hydrogen silicone oil of 0.2-2.0% with hydrogeneous matrix amount percentage, containing hydrogen silicone oil accounts for the mass percent 30% and the double bond containing polyoxyethylene of end group of reaction raw materials, the polyethers of polyoxypropylene block polymerization, polyethers accounts for the mass percent 70% of reaction raw materials, above-mentioned raw materials is added in the flask, be warming up to 60 degree, the platinum chloric acid or the trifluoroacetic acid that add the quality 100ppm that accounts for reaction raw materials carry out catalysis, then under 100-120 degree temperature, through hydrosilylation, 4-5 hour and make;
Described polyether modified silicon oil also can directly be bought, the key technical indexes: the light yellow transparent oily liquid of outward appearance; Temperature is in the time of 25 ℃, and density is 1.03 g/cm
3Viscosity is 1500 ~ 4000CS; Cloud point is 47 ℃; Effective ingredient 〉=99.5%.
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| CN103572653A (en) * | 2013-10-31 | 2014-02-12 | 江苏赛欧信越消泡剂有限公司 | Emulsion type silicon resin defoaming agent for pulping in papermaking |
| CN104069654A (en) * | 2014-07-01 | 2014-10-01 | 西安道尔达化工有限公司 | Preparation method of high-viscosity organic silicon defoamer |
| CN104492127A (en) * | 2014-12-04 | 2015-04-08 | 宿州市华润化工有限责任公司 | Method for preparing preservative-free organic silicone defoamer |
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