CN105031978B - A kind of silicon ether composite anti-foaming agent emulsion and preparation method thereof - Google Patents
A kind of silicon ether composite anti-foaming agent emulsion and preparation method thereof Download PDFInfo
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- CN105031978B CN105031978B CN201510535129.7A CN201510535129A CN105031978B CN 105031978 B CN105031978 B CN 105031978B CN 201510535129 A CN201510535129 A CN 201510535129A CN 105031978 B CN105031978 B CN 105031978B
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000000839 emulsion Substances 0.000 title claims abstract description 43
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 27
- 239000010703 silicon Substances 0.000 title claims abstract description 27
- 239000002518 antifoaming agent Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002131 composite material Substances 0.000 title claims abstract description 10
- 238000004945 emulsification Methods 0.000 title description 4
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- -1 allyl ether modified silicon Chemical class 0.000 claims abstract description 14
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 9
- 239000003921 oil Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 7
- 229920002545 silicone oil Polymers 0.000 claims abstract description 7
- 238000000265 homogenisation Methods 0.000 claims abstract description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims description 8
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 7
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 5
- 229940083466 soybean lecithin Drugs 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000855 fermentation Methods 0.000 abstract description 16
- 230000004151 fermentation Effects 0.000 abstract description 16
- 239000013530 defoamer Substances 0.000 abstract description 15
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 230000002045 lasting effect Effects 0.000 abstract description 3
- 230000000813 microbial effect Effects 0.000 abstract description 2
- 244000005700 microbiome Species 0.000 abstract description 2
- 239000006260 foam Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 8
- 229920000570 polyether Polymers 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- 235000019241 carbon black Nutrition 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 235000010469 Glycine max Nutrition 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 2
- 238000012644 addition polymerization Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000000787 lecithin Substances 0.000 description 2
- 235000010445 lecithin Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Degasification And Air Bubble Elimination (AREA)
Abstract
The invention discloses a kind of silicon ether composite anti-foaming agent emulsion, its is composed of the following components：Linear dimethyl silicone oil, allyl ether modified silicon oil, polypropylene glycerol aether, modified white carbon black, triethanolamine and compound emulsifying agent；Its preparation method is：Linear dimethyl silicone oil is uniformly mixed with modified white carbon black, heated；Triethanolamine is added, is cooled down after stirring；Allyl ether modified silicon oil and polypropylene glycerol aether are added, continues to stir；Compound emulsifying agent high-speed stirred is added, forms thick emulsion；Viscous water is added in thick emulsion, configures emulsion；Emulsion is poured into high-speed homogenization machine and stirred, forms fine and smooth stable microemulsion.The defoamer is easily dispersed in water, and specific surface area is small, and defoaming is quick and suds are lasting, and dosage is few；Preparation method simplicity is easily operated；This defoamer acts on for microorganism nonhazardous, and can promote mycelial growth, beneficial to microbial fermentation, more environmentally friendly.
Description
Technical field
The present invention relates to a kind of preparation method for defoaming agent emulsion, more particularly to a kind of system of silicon ether composite anti-foaming agent emulsion
Preparation Method.
Background technology
In the production of most of fermentation industries, a large amount of foams are often produced, the presence of foam can have a strong impact on product
Quality, even resulting in production can not be normally carried out；It is a kind of not only easy but also economic defoaming mode to add defoamer, at present
It is widely used in the every field of fermentation.Commodity defoamer is various in style both at home and abroad, different properties, is broadly divided into from composition
Three classes, i.e. organic silicon type, polyether-type and grease type, defoamer application field is extensive, therefore is increasingly paid attention to by every profession and trade.Oil
The defoamer of lipid is although relatively inexpensive, but suds ability is poor, and defoamed ratio is low, is not easy to disperse in aqueous phase, applicable surface is narrow.It is poly-
Ethers defoamer has good water-soluble, and suds ability is stronger, is widely used in fermentation industry, but its defoaming effectiveness
Low, cost is higher.Organic silicon defoamer has excellent defoaming, chemical stability, physiological inertia, cold resistance and heat resistance,
But due to its bad water solubility, it is necessary to it could be used using the emulsifier of costliness, but the defoaming of its emulsion and suds
Ability all receives great infringement, and its emulsion is also unstable, easily demulsification, and these limit its use in fermentation industry.
With the development of defoamer, some new high activity defoaming components are constantly found, compounding component synergistic effect is studied continuous
Deeply, the low-grade defoamer that those component structures are single, economic benefit is poor gradually compound will be disappeared by multi-functional, efficient
Infusion substitutes, and develops strong applicability, and dosage is small, and the new and effective defoamer that can improve product quality and utilization rate of equipment and installations will be worked as
The developing direction of primary fermentation industry defoamer.
The content of the invention
In order to solve the above technical problems, the present invention proposes a kind of silicon ether composite anti-foaming agent emulsion and preparation method thereof, its energy
The maximum capacity of defoaming effective active matter is given full play to, gropes optimum formula by many experiments, makes it in fermentation system
Possess quick defoaming capacity and lasting suds ability.
In order to achieve the above object, technical scheme is as follows：A kind of silicon ether composite anti-foaming agent emulsion, by weight hundred
Divide than composed of the following components：
Further, it is composed of the following components by weight percentage：
A kind of preparation method of silicon ether composite anti-foaming agent emulsion, comprises the following steps：
(1) 100~150 parts of linear dimethyl silicone oil are uniformly mixed with 0~5 part of modified white carbon black, is heated to 130 DEG C；
(2) 3~5 parts of triethanolamines are added in step (1), after stirring 3h, are cooled to 80 DEG C~100 DEG C；
(3) 30~50 parts of allyl ether modified silicon oils and 20~40 parts of polypropylene glycerol aethers are added, continue to stir 1h；
(4) then, 7~12 parts of compound emulsifying agent high-speed stirreds are added, form thick emulsion；
(5) 320ml~480ml is added in the thick emulsion of step (4), mass concentration is 0.3%~1% viscous water, is matched somebody with somebody
Put the emulsion that solid content is 20%~35%；
(6) emulsion in step (5) is poured into high-speed homogenization machine, high-speed stirred is carried out with 12000r/min, stirs 20-
25min, form fine and smooth stable microemulsion.
Preferably, the compound emulsifying agent added in step (4) is Tween-80 and the compound of soybean lecithin, its
By Tween-80:Soybean lecithin=1:1 ratio mixing, make the HLB value of compound emulsifying agent 10 or so, so after emulsification
Silicon ether emulsion is more stable.
Preferably, the viscous water is hydroxymethyl cellulose viscous water, because hydroxymethyl cellulose wide material sources, to people
Body is harmless, belongs to environmentally friendly thickening material, so selecting hydroxymethyl cellulose viscous water in this patent.
Beneficial effects of the present invention：
(1) it is easily dispersed in water, specific surface area is small, and defoaming is quick and suds are lasting, and dosage is few；
(2) compare with conventional fermented type polyether antifoam agent, the method for preparing this defoamer, it is easy to be easily operated；
(3) this defoamer acts on for microorganism nonhazardous, and can promote mycelial growth, has to microbial fermentation
Benefit；
(4) this defoamer is produced, does not produce waste water, waste gas, reduces the processing of substantial amounts of debirs, greatly reduces
Cost, it is beneficial to largely produce, it is more environmentally friendly；
(5) stability of emulsion is more stable compared with general organic silicon emulsion, chemical property more inertia, is not easy with being typically situated between
Matter reacts.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.
It is related to specific number in the present invention, refers to parts by weight：
Embodiment one
100 parts of linear dimethyl silicone oil uniformly mix with 3 parts of modified white carbon blacks, and heating-up temperature is to 130 DEG C；Add 3 part three
Monoethanolamine, after stirring 3 hours, it is cooled to 90 °；40 parts of allyl ether modified silicon oils and 25 parts of polypropylene glycerol aethers are added, after
After continuous stirring one hour；Add 10 parts of compound emulsifying agent high-speed stirreds, form thick emulsion, wherein compound emulsifying agent by 5 parts of tweens-
80 and 5 parts of soybean lecithins mix；Increase then to the hydroxymethyl cellulose for 320mL being added in thick emulsion, concentration is 0.5%
Thick water, configure the emulsion of 35% solid content；Then this emulsion is poured into high-speed homogenization machine, high-speed stirring is carried out with 12000r/min
20min is mixed, forms fine and smooth stable microemulsion；This microemulsion can guarantee that in 5000r/min centrifuges centrifuge 5min and regardless of
Layer.
Test method：100mL foam liquids are poured into 500mL graduated cylinders, the glass tube being connected with air pump is inserted into foam liquid
Middle bubbling, it is 3L/min to control the air capacity being passed through, and observes the foaming situation in graduated cylinder, is carved when foam rapidly rises to 500mL
When spending line, stop bubbling, the defoaming agent emulsion that 50 μ L are prepared, while timing are added dropwise into foam liquid, record foam drops to
The time of 110mL graduation marks, this time are defined as foam time, embody defoaming capacity, then proceed to bubbling, and timing is simultaneously observed
Foam lifting height, the graduation mark of foam when recording 30min, secondary height are defined as suds ability.And with organic silicon emulsion, poly-
The foam time and suds ability of ether and fatty acid amide are contrasted, and specific experimental data is as shown in Table 1：
Table one：
| Product type | Organic silicon emulsion | Polyethers | Fatty acid amide | Silicon ether |
| Foam time (s) | 15 | 27 | 25 | 8 |
| Suds ability (mL) | 240 | 210 | 270 | 160 |
It was found from table results, this product either defoaming capacity or suds ability are superior to existing in the market similar
Product.
Embodiment two
100 parts of linear dimethyl silicone oil uniformly mix with 5 parts of modified white carbon blacks, and heating-up temperature is to 130 DEG C；Add 5 part three
Monoethanolamine, after stirring 3 hours, it is cooled to 80 °；50 parts of allyl ether modified silicon oils and 35 parts of polypropylene glycerol aethers are added,
Continue to stir 1h；7 parts of compound emulsifying agent high-speed stirreds are added, form thick emulsion, wherein compound emulsifying agent is by 3.5 parts of Tween-80s
Mixed with 3.5 parts of soybean lecithins；Increase then to the hydroxymethyl cellulose for 360mL being added in thick emulsion, concentration is 0.5%
Thick water, configure the emulsion of 35% solid content；Then this emulsion is poured into high-speed homogenization machine, high-speed stirring is carried out with 12000r/min
25min is mixed, forms fine and smooth stable microemulsion；This microemulsion can guarantee that in 5000r/min centrifuges centrifuge 5min and regardless of
Layer.
Test method：35kg fermentation liquor bed charges, 50L fermentation tanks, addition 5g polyether antifoam agent, 10h first into bed material
Afterwards, stream addition polymerization ether defoaming agent, suds time are 15min for the first time, a fermentation period dosage 20g, acid production rate 22%.Same
In environment, the silicon ether defoaming agent of the above-mentioned preparations of 5g is added in bed material, after 15h, for the first time stream plus silicon ether defoaming agent, suds time be
40min, a fermentation period dosage 16g, acid production rate 24%.Its data is as shown in Table 2：
Table two：
| Product type | Polyethers | Silicon ether |
| The suds time (min) | 15 | 40 |
| Product dosage (g) | 20 | 16 |
| Acid production rate (%) | 22 | 24 |
| Solid content (%) | 100 | 35 |
This it appears that the silicon ether defoaming agent that we prepare has the longer suds time, total amount of adding is less for this experiment,
Silicon ether defoaming agent is beneficial to the growth of mycelia, and sour yield is higher.
Embodiment three
100 parts of linear dimethyl silicone oil uniformly mix with 3 parts of modified white carbon blacks, and heating-up temperature is to 130 DEG C；Add 2 part three
Monoethanolamine, after stirring 3h, it is cooled to 80 DEG C；30 parts of allyl ether modified silicon oils and 30 parts of polypropylene glycerol aethers are added, after
Continuous stirring 1h；8 parts of compound emulsifying agent high-speed stirreds are added, form thick emulsion, wherein compound emulsifying agent is by 4 parts of Tween-80s and 4 parts
Soybean lecithin mixes；Thickened then to the hydroxymethyl cellulose for 480mL being added in thick emulsion, mass concentration is 0.3%
Water, configure the emulsion of 25% solid content；Then this emulsion is poured into high-speed homogenization machine, high-speed stirred is carried out with 12000r/min
20min, form fine and smooth stable microemulsion；This microemulsion can guarantee that in 3000r/min centrifuges centrifuge 5min and it is not stratified.
Test method：35kg fermentation liquor bed charges, 50L fermentation tanks, addition 5g polyether antifoam agent, 10h first into bed material
Afterwards, stream addition polymerization ether defoaming agent, suds time are 15min for the first time, a fermentation period dosage 20g, acid production rate 22%.Same
In environment, the silicon ether defoaming agent of the above-mentioned preparations of 5g is added in bed material, after 15h, for the first time stream plus silicon ether defoaming agent, suds time be
15min, a fermentation period dosage 21g, acid production rate 23%.Its concrete numerical value is referring to table three：
Table three：
| Product type | Polyethers | Silicon ether |
| The suds time (min) | 15 | 15 |
| Product dosage (g) | 20 | 21 |
| Acid production rate (%) | 22 | 23 |
| Solid content (%) | 100 | 25 |
Even if this experiment it can be seen that reduce silicon ether defoaming agent solid content, its suds time, total amount of adding also with it is similar
Polyether antifoam agent effect is suitable, and growth of the silicon ether defoaming agent to mycelia in addition has facilitation, makes sour yield higher.
Claims (3)
1. a kind of silicon ether composite anti-foaming agent emulsion, it is characterised in that composed of the following components by weight percentage：
2. silicon ether composite anti-foaming agent emulsion according to claim 1, it is characterised in that by weight percentage by following components
Composition：
3. a kind of preparation method of silicon ether composite anti-foaming agent emulsion, it is characterised in that comprise the following steps：
(1) 100~150 parts of linear dimethyl silicone oil are uniformly mixed with 0~5 part of modified white carbon black, is heated to 130 DEG C；
(2) 3~5 parts of triethanolamines are added in step (1), after stirring 3h, are cooled to 80 DEG C~100 DEG C；
(3) 30~50 parts of allyl ether modified silicon oils and 20~40 parts of polypropylene glycerol aethers are added, continue to stir 1h；
(4) then, 7~12 parts of compound emulsifying agent high-speed stirreds are added, form thick emulsion, the compound emulsifying agent is Tween-80
With the compound of soybean lecithin, it presses Tween-80:Soybean lecithin=1:1 ratio mixing；
(5) 320ml~480ml is added in the thick emulsion of step (4), mass concentration is 0.3%~1% viscous water, and configuration is solid
Content is 20%~35% emulsion, and the viscous water is hydroxymethyl cellulose viscous water；
(6) emulsion in step (5) is poured into high-speed homogenization machine, high-speed stirred is carried out with 12000r/min, stirs 20-
25min, form fine and smooth stable microemulsion.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106799068A (en) * | 2016-12-27 | 2017-06-06 | 广东中联邦精细化工有限公司 | A kind of special defoamer of food and preparation method |
| CN108159737B (en) * | 2017-12-07 | 2020-06-23 | 中海油天津化工研究设计院有限公司 | Defoaming agent for wet-process phosphoric acid production and preparation method thereof |
| CN111979834A (en) * | 2020-09-01 | 2020-11-24 | 南京鼎兆新材料技术研发有限公司 | Preparation method of modified silicone oil type papermaking defoaming agent |
| CN113144678A (en) * | 2020-12-09 | 2021-07-23 | 金湖金凌新材料科技有限公司 | Composite defoaming agent with lasting foam inhibition performance and preparation method thereof |
| CN113350834A (en) * | 2021-05-27 | 2021-09-07 | 中石化重庆页岩气有限公司 | Foaming defoaming agent for normal-pressure shale gas development and preparation method thereof |
| CN114618190A (en) * | 2022-03-31 | 2022-06-14 | 山东师范大学实验厂 | A kind of high temperature resistant silicone emulsion type defoamer and preparation method thereof |
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| CN1031489C (en) * | 1992-12-14 | 1996-04-10 | 旅顺联营化工厂 | strong defoaming agent |
| CN1283348C (en) * | 2005-01-05 | 2006-11-08 | 长春理工大学 | Organic silicon ether defoaming agent for food processing |
| CN102120159A (en) * | 2010-11-19 | 2011-07-13 | 苏州博纳化学科技有限公司 | Method for preparing emulsified silicone oil defoamer |
| CN102160939B (en) * | 2011-03-02 | 2013-08-14 | 江苏斯德瑞克化工有限公司 | Self-emulsifying molecular antifoaming agent and preparation method thereof |
| CN102961896B (en) * | 2011-11-17 | 2014-09-03 | 天津法莫西医药科技有限公司 | Powder defoaming agent with flyash hollow glass beads as filler |
| CN102716599B (en) * | 2012-07-03 | 2014-01-01 | 保利民爆济南科技有限公司 | Production technology of silyl ether defoaming agent for fermentation process |
| CN102949867A (en) * | 2012-09-19 | 2013-03-06 | 天津科创医药中间体技术生产力促进有限公司 | High-efficiency antifoaming agent |
| CN103028275B (en) * | 2012-12-25 | 2014-12-17 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation method of solid organic silicon defoamer |
| 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 |
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