CN105498303B - A kind of organic silicon defoamer and preparation method thereof - Google Patents
A kind of organic silicon defoamer and preparation method thereof Download PDFInfo
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- CN105498303B CN105498303B CN201510925719.0A CN201510925719A CN105498303B CN 105498303 B CN105498303 B CN 105498303B CN 201510925719 A CN201510925719 A CN 201510925719A CN 105498303 B CN105498303 B CN 105498303B
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- defoamer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0418—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing P-atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0422—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing S-atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0431—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance containing aromatic rings
- B01D19/0436—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance containing aromatic rings with substituted groups
- B01D19/0454—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance containing aromatic rings with substituted groups which contain S-atoms
Abstract
The invention belongs to defoamer and preparing technical field, is related to a kind of complex type organic silicon defoamer and preparation method thereof, each component percentage by weight is in organic silicon defoamer：Distilled water 48% 54%, silica 1 .1% 2.48%, dimethicone 38% 48.5%, emulsifying agent 1% 3%, assistant for emulsifying agent 1% 6%, stabilizer 0.5% 1%, total weight percent 100%；During preparation, main defoamer first is made with silica and dimethicone, then adding distilled water, assistant for emulsifying agent, emulsifying agent and stabilizer into reaction unit in proportion successively adds main defoamer emulsification to after being completely dissolved, that is, obtains organic silicon defoamer；Its preparation technology is simple, and raw material is easy to get, and cost is low, the organic silicon defoamer of preparation while good antifoaming performance is kept, have the characteristics that efficiently, stably, it is alkaline-resisting and heat-resisting.
Description
Technical field：
The invention belongs to defoamer and preparing technical field, is related to a kind of complex type organic silicon defoamer and its preparation side
Method.
Background technology：
Since German experimental physicist Quincke proposes chemically, to defoam, up to the present to have undergone first
Four updates.First generation defoamer is that mineral oil, aliphatic acid and fatty acid ester, fatty acid amide, lower alcohols etc. are organic
Thing, this organic defoamer is cheap, is still largely using in the market, but the elimination ability to dense form foam compared with
Difference；Second generation defoamer is polyethers defoamer, mainly has straight-chain polyether and is esterified by alcohol, ammonia for the polyethers or end group of initiator
Polyether derivative, suds ability is stronger, is the leading defoamer of current fermentation industry application, but brokenly bubble rate it is low, it is necessary to newly plus
A certain amount of defoamer, in order to adapt to defoaming requirement and the changeable situation of operating condition, develop organic silicon defoamer i.e. the 3rd
For defoamer, organic silicon defoamer is generally dimethyl silicone polymer, and dimethicone belongs to the poly- methyl of line style of MDnM types
Siloxanes, it is the "the" shape chain of easy flexing in molecule, this defoamer defoaming effectiveness is very high, but suds effect has the time difference strong
People's will.Thus, organosilicon can be with other surfactant compounds for having defoaming, suds active such as fatty acid amide, polyethers
Into composite anti-foaming agent, the suds ability of organic silicon defoamer so can be both improved, and can reduces the cost of product.Forth generation disappears
Infusion is Siloxane-Oxyalkylene Copolymers class defoamer, is to introduce polyether segment by modified on polysiloxanes segment.It is this kind of to disappear
Infusion high temperature resistant, strong basicity resisting, can be rapid soluble in water, can be used alone, can be also used cooperatively with other inorganic agents, stability
It is good, the floating oil phenomenon that is demulsified does not occur, also deposit-free produces, also effective to non-aqueous system.Chinese patent CN103074784 is proposed
A kind of composite organic defoamer using starch as stabilizer, add the stability of product, can prevent from condensing, be demulsified it is existing
The generation of elephant, but because the dosage of stabilizer is larger so that antifoaming performance is deteriorated；Chinese patent CN104225965 is proposed
Emulsion-type organic silicon defoamer using high boiling point silicon oil as one of raw material, reduces production cost, is that organic silicon monomer by-product is high
Boiling thing processing provides rational processing channel；With polyvinyl alcohol (PVA) for thickener, but in water dissolved title, can produce
Foam, production capacity is reduced, influence quality and the use of product；What Chinese patent CN103603215 was proposed is to pass through addition
Organotin catalysts make silicone particles be not easy to split in the interruption of strong acid alkali systems, and product can use under severe conditions, but raw
Production cost is higher, and preparation technology is more complicated；CN103830938 is proposed using nonionic surfactant as emulsifying agent, can be with
Be in Tween-60, Arlacel-40 or polyether silicone oil at least any one, emulsifying capacity is higher, but product alkali resistance it is poor and
Cost is higher.
The content of the invention
The shortcomings that it is an object of the invention to overcome prior art to exist, seek design provide a kind of organic silicon defoamer and
Its preparation method, the organic silicon defoamer of preparation also have preferably stable while with strong defoaming with strong suds ability
Property, good anti-dilution capacity and wider pH and temperature applicable range.
To achieve these goals, organic silicon defoamer of the present invention includes distilled water, dimethicone, titanium dioxide
Silicon, emulsifying agent, assistant for emulsifying agent and stabilizer；Its each component percentage by weight is：Distilled water 48%-54%, silica
1.1%-2.48%, dimethicone 38%-48.5%, emulsifying agent 1%-3%, assistant for emulsifying agent 1%-6%, stabilizer 0.5%-
1%, total weight percent 100%.
Emulsifying agent of the present invention is anion surfactant, is dodecyl sodium sulfate or DBSA
Sodium.
Assistant for emulsifying agent of the present invention is the one or two of AEO-9 and tributyl phosphate, its hydrophilic lipophilic balance
(HLB) it is 7~9.
Stabilizer of the present invention is sanlose 800~1200.
The specific preparation process of organic silicon defoamer of the present invention is：
(1), the preparation of main defoamer：In the reaction unit of the heating of existing band and agitating function, 3-5 mass parts are added
Silica solid powder, the dimethicone of 100 mass parts is slowly added under agitation, reacted under 180 DEG C of temperature conditionss
Main defoamer of good performance (silicon cream) is made in 3h, by main defoamer be cooled to 80 DEG C it is standby；
(2), compound emulsion：Added in the reaction unit of the heating of existing band and agitating function and account for product population 48%-
54% distilled water, and 80 DEG C are heated to, then sequentially add 1%-6% assistant for emulsifying agents, 1%-3% emulsifying agents and 0.5%-
1% stabilizer, mixed solution is obtained after being completely dissolved, be slowly added dropwise into mixed solution and be cooled to 80 DEG C and account for product gross weight
40%-48% main defoamer (silicon cream) is simultaneously sufficiently stirred, and stops heating after emulsifying 0.5-1h, room is naturally cooled to after homogeneous
Temperature, obtain the organic silicon defoamer of thick white emulsion form.
The present invention compared with prior art, by using dimethicone as raw material, adds auxiliary agent silica, silica
Surface hydroxyl is advantageous to the scattered of silicone oil, can improve the antifoam performance of silicone oil；Due to the good surface for reducing water
Power, wetting, infiltration and emulsification anion surfactant addition so that the foaming power of emulsifying agent it is smaller and with compared with
Good emulsifying capacity.Simultaneously by the compounding of various emulsifying agents, there are AEO-9, dodecyl sodium sulfate or DBSA
Sodium, sanlose 800~1200 (CMC) and tributyl phosphate, enhance the balance and stably of hydrophilic and oleophilic system
Property, the combination property of emulsion is improved, it is such as alkaline-resisting, heat-resisting.In addition, addition thickener sanlose 800~
1200 (CMC) improve the viscosity of decentralized medium, further increase emulsion intercalation method；Its preparation technology is simple, and raw material is easy
, cost is low, the organic silicon defoamer of preparation while good antifoaming performance is kept, have it is efficient, stably, it is alkaline-resisting and resistance to
The features such as hot.
Embodiment：
Below by embodiment, the invention will be further described.
Embodiment 1：
The process that the present embodiment prepares organic silicon defoamer is：
(1) preparation of the main defoamers of：In the reaction unit of the heating of existing band and agitating function, the two of 3 parts of quality is added
Silica solids powder, the dimethicone of 100 parts of quality is slowly added under agitation, reacted under about 180 DEG C of temperature conditionss
3h, that is, be made main defoamer (silicon cream) of good performance, by main defoamer be cooled to 80 DEG C or so it is standby；
(2) preparation of defoamers：The distilled water for accounting for final products gross mass 49% is added into existing band heating and stirring work(
Can reaction unit in and be heated to 80 DEG C, sequentially add 2% dodecyl sodium sulfate, 2.5% tributyl phosphate,
0.8% sanlose 800~1200 (CMC) and 2.2% AEO-9,43.5% is added until completely dissolved
Main defoamer, it is warm and stirred in 2000r/min or so, its is stopped stirring after fully emulsified 50 minutes and be cooled to room
Temperature, obtain the organic silicon defoamer that form is thick white emulsion.
The process that the present embodiment prepares organic silicon defoamer is：
(1) preparation of the main defoamers of：In the reaction unit of the heating of existing band and agitating function, the two of 5 parts of quality is added
Silica solids powder, the dimethicone of 100 parts of quality is slowly added under agitation, reacted under about 180 DEG C of temperature conditionss
3h, that is, be made main defoamer (silicon cream) of good performance, by main defoamer be cooled to 80 DEG C or so it is standby；
(2) preparation of defoamers：The distilled water for accounting for final products gross mass 54% is added into existing band heating and stirring work(
Can reaction unit in and be heated to 80 DEG C, sequentially add 2.2% dodecyl sodium sulfate, 2.5% tributyl phosphate,
0.6% sanlose 800~1200 (CMC) and 0.7% AEO-9,40% master is added until completely dissolved
Defoamer, it is warm and stirred in 2000r/min or so, its is stopped stirring after fully emulsified 60 minutes and be cooled to room temperature,
Obtain the organic silicon defoamer that form is thick white emulsion.
Embodiment 3：
The process that the present embodiment prepares organic silicon defoamer is：
(1) preparation of the main defoamers of：In the reaction unit of the heating of existing band and agitating function, the two of 3 parts of quality is added
Silica solids powder, the dimethicone of 100 parts of quality is slowly added under agitation, reacted under about 180 DEG C of temperature conditionss
3h, that is, be made main defoamer (silicon cream) of good performance, by main defoamer be cooled to 80 DEG C or so it is standby；
(2) preparation of defoamers：The distilled water for accounting for final products gross mass 50% is added into existing band heating and stirring work(
Can reaction unit in and be heated to 80 DEG C, sequentially add 1% neopelex, 3% tributyl phosphate and
0.8% sanlose 800~1200 (CMC), 45.2% main defoamer is added until completely dissolved, it is warm
And stirred in 2000r/min or so, make its stop stirring after fully emulsified 30 minutes and be cooled to room temperature, obtain form as white
The organic silicon defoamer of viscous emulsion.
Embodiment 4：
The process that the present embodiment prepares organic silicon defoamer is：
(1) preparation of the main defoamers of：In the reaction unit of the heating of existing band and agitating function, the two of 4 parts of quality is added
Silica solids powder, the dimethicone of 100 parts of quality is slowly added under agitation, reacted under about 180 DEG C of temperature conditionss
3h, that is, be made main defoamer (silicon cream) of good performance, by main defoamer be cooled to 80 DEG C or so it is standby；
(2) preparation of defoamers：The distilled water for accounting for final products gross mass 52% is added into existing band heating and stirring work(
Can reaction unit in and be heated to 80 DEG C, sequentially add 3% neopelex, 1% tributyl phosphate,
0.5% sanlose 800~1200 (CMC) and 3% AEO-9,40.5% master is added until completely dissolved
Defoamer, it is warm and stirred in 2000r/min or so, its is stopped stirring after fully emulsified 40 minutes and be cooled to room temperature,
Obtain the organic silicon defoamer that form is thick white emulsion.
Embodiment 5：
The process that the present embodiment prepares organic silicon defoamer is：
(1) preparation of the main defoamers of：In the reaction unit of the heating of existing band and agitating function, the two of 3 parts of quality is added
Silica solids powder, the dimethicone of 100 parts of quality is slowly added under agitation, reacted under about 180 DEG C of temperature conditionss
3h, that is, be made main defoamer (silicon cream) of good performance, by main defoamer be cooled to 80 DEG C or so it is standby；
(2) preparation of defoamers：The distilled water for accounting for final products gross mass 49.5% is added into existing band heating and stirring
In the reaction unit of function and it is heated to 80 DEG C, sequentially adds 2.2% neopelex, 2.5% tricresyl phosphate
Butyl ester, 0.6% sanlose 800~1200 (CMC) and 2.2% AEO-9, are added until completely dissolved
40.5% main defoamer, it is warm and 2000r/min or so stir, make its stops after fully emulsified 30 minutes stir and it is cold
But room temperature is arrived, obtains the organic silicon defoamer that form is thick white emulsion.
Optimum condition prepared by the present embodiment organic silicon defoamer：HLB between 7~9, whipping temp at 80 DEG C or so,
Mixing speed is in 2000r/min or so.
The present embodiment the organic silicon defoamer of preparation is carried out respectively stabilization, alkaline-resisting, resistance to ATSC (acetone semicarbazone thiocarbamide),
Antifoam performance test under antifoaming speed, heat-resisting and alkalescence condition, it is specially：
(1) dewatering ability is tested：Centrefuge experiment is carried out with 3000r/min to product and sample, testing time 20min is not
Layering；
(2) alkaline-resisting test：It is 5% mixed aqueous solution by defoaming agent emulsion, the sodium hydroxide mass fraction of preparation
80mL is placed in 100mL beakers, is stood after being stirred ten minutes with magnetic stirrer under high shear, solution after observing 24 hours
Character, not wax deposition；
(3) resistance to ATSC (acetone semicarbazone thiocarbamide) test：Organic silicon defoamer, sodium hydroxide and ATSC weight percents are contained
Amount is that 5% mixed aqueous solution 80mL is placed in 100mL beakers, after being stirred ten minutes with magnetic stirrer under high shear
Stand, the character of solution, not stratified, not wax deposition after observation 24 hours；
(4) antifoaming speed is tested：It is standby that made defoamer and water are made into the dilution containing defoamer 1%, by bubbler
Core is put into 500mL graduated cylinders, add percentage containing surfactant qualities be 1% foam liquid to 200mL scales, start air pump
Bubbling, stop bubbling when foam height rises to 500mL, it is 1% that the mass percent that 25mL is configured is injected in graduated cylinder
The timing simultaneously of defoaming agent solution dilution, be foam time during to lather collapse, be repeated 3 times and average；
(5) resistance to Thermal test：The organic silicon defoamer of preparation is taken to be placed in test tube in baking oven, when temperature rises to 110
DEG C when start timing, cooled after 2 hours to room temperature, take out sample observation resistance to elevated temperatures；
(6) the defoaming test under alkalescence condition：PH=14 percentage containing surfactant qualities is added in 100mL graduated cylinders
Number shakes 30 times for 1% foam liquid foam liquid 50mL, and the rear 0.2mL that adds is made into the dilution containing defoamer 1% by defoamer
Organic silicon defoamer measures remaining foam volume.
Claims (1)
1. a kind of preparation method of organic silicon defoamer, it is characterised in that specifically preparation process is：
(1) preparation of the main defoamers of：In the reaction unit of the heating of existing band and agitating function, the titanium dioxide of 3 parts of quality is added
Silicon solid powder, the dimethicone of 100 parts of quality is slowly added under agitation, react 3h under about 180 DEG C of temperature conditionss, i.e.,
Be made main defoamer of good performance, by main defoamer be cooled to 80 DEG C it is standby；
(2) preparation of defoamers：The distilled water for accounting for final products gross mass 49% is added into existing band heating and agitating function
In reaction unit and be heated to 80 DEG C, sequentially add 2% dodecyl sodium sulfate, 2.5% tributyl phosphate, 0.8%
Sanlose 800~1200 and 2.2% AEO-9, until completely dissolved add 43.5% main defoamer, warp
It is incubated and is stirred in 2000r/min, make its stop stirring after fully emulsified 50 minutes and be cooled to room temperature, obtains form as white
The organic silicon defoamer of viscous emulsion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110548315A (en) * | 2019-08-14 | 2019-12-10 | 湖南登科材料科技有限公司 | Novel organic silicon defoaming agent and preparation method thereof |
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101987256A (en) * | 2009-08-02 | 2011-03-23 | 扬州润达油田化学剂有限公司 | Production process of organosilicone emulsion defoaming agent |
| CN103877755B (en) * | 2014-03-11 | 2016-03-02 | 苏州恒康新材料有限公司 | A kind of silicone defoaming agent and preparation method thereof |
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| CN110548315A (en) * | 2019-08-14 | 2019-12-10 | 湖南登科材料科技有限公司 | Novel organic silicon defoaming agent and preparation method thereof |
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