CN105152255A - Preparation method of defoaming agent for wastewater treatment - Google Patents
Preparation method of defoaming agent for wastewater treatment Download PDFInfo
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- CN105152255A CN105152255A CN201510607976.XA CN201510607976A CN105152255A CN 105152255 A CN105152255 A CN 105152255A CN 201510607976 A CN201510607976 A CN 201510607976A CN 105152255 A CN105152255 A CN 105152255A
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Abstract
The invention discloses a preparation method of a defoaming agent for wastewater treatment, and belongs to the field of water treatment agents. The preparation method of the defoaming agent comprises the following steps of organic silicone oil modification treating, silicone paste preparing and defoaming agent compounding. The defoaming agent is prepared by compounding the organic silicone oil which is good in chemical stability and is modified through polyether with silicone paste, emulsifying auxiliaries and the like. The defoaming agent is high in chemical stability and defoaming and anti-foaming capacity, capable of resisting strong acid and strong base, small in additive amount and long in anti-foaming time, and the COD of wastewater can not be increased, so that wastewater secondary pollution caused by defoaming agent adding can be avoided.
Description
Technical field
The invention belongs to water conditioner field, be specifically related to a kind of preparation method of use in waste water treatment defoamer.
Background technology
In wastewater treatment process, easily produce a large amount of foam, need to eliminate in time, general regular interpolation defoamer.Current defoamer is mainly divided three classes: mineral oils, silicone based, polyethers.Common defoamer poor chemical stability, and complicated component in waste water, cause common defoamer floating oil, foam time is short.
The research of defoamer in recent years mainly concentrates on the Compositional type defoamer such as composite of composite, the polyethers of silicoorganic compound and tensio-active agent and organosilyl composite, water-soluble or oil soluble polyethers and silicon-containing polyether.With regard to current defoamer, the performance of polyethers and silicone based defoamer is the most excellent, to the modification of this two defoamer and the development research of new variety also more active.
Patent No. ZL200410064717.9 discloses a kind of high-temperature defoamer and preparation method thereof, and it is made up of following component: (1) defoaming activity material: comprise organic poly-silicon gas alkane, hydrophobic silicic aerogels, polyoxyethylene and polyoxypropylene block polymer; (2) emulsifying agent, organosilyl surfactant; (3) dispersion medium water.The preparation method of this high-temperature defoamer comprises the following steps: that (1) emulsifying agent first mixes with defoaming activity thing; (2) at 50 ~ 80 DEG C of abundant mix and blends, water is added in oil and carry out phase inversion; (3) mixture after phase inversion in step (2) is entered colloidal mill circulation, redilution can obtain high-temperature defoamer.This high-temperature defoamer, at middle high-temperature (60 ~ 90 DEG C), has good antifoaming performance and stability; In high temperature Jet Overflow dye process, still can keep good antifoaming performance and stability, the defect of dyeing inequality or specking can not be caused.
Patent No. ZL200510034583.0 discloses a kind of preparation method of industrial defoaming agent, its method first glycerine is aggregated into the polyglycerol that the polymerization degree is 2-10 under catalysts conditions, then adds glycerol fatty acid ester by definite quality ratio or lipid acid carries out transesterify.This invention production technique is easy, and raw material is easy to get, froth breaking, press down bubble effective, be applicable to the techniques such as papermaking, sugaring, fermentation.
Patent No. ZL200410027790.9 discloses water insoluble defoamer and preparation method thereof of a kind of Nano/micron grade silicon dioxide synthesis, and this defoamer be 5 ~ 2000nm is 1200 ~ 2600 without the silicon-dioxide of hydrophobic treatment, the molecular weight interpolymer that is 800 ~ 2000, the molecular weight dimethyl silicone oil that is 15000 ~ 60000, polyoxyethylene (4 ~ 10) octylphenol ether, molecular weight by particle diameter propylene glycol polyoxyethylene poly-oxygen propylene aether forms; The preparation method of above-mentioned defoamer, comprises the following steps: silicon-dioxide to carry out pyroprocessing; By the silicon-dioxide after pyroprocessing and dimethyl silicone oil stirring reaction, then add interpolymer, after continuing reaction, pump water and the ethanol of reaction generation; Add polyoxyethylene (4 ~ 10) octylphenol ether and propylene glycol polyoxyethylene poly-oxygen propylene aether, pump water and the ethanol of reaction generation after continuing reaction, be naturally down to room temperature.This invention defoaming effect is good, stable performance, is suitable for applying in high-efficient cutting grinding coolant.
Patent No. ZL01144354.5 discloses a kind of emulsion type defoaming agent, and this defoamer is the C by the alkymer of 40 ~ 60 mass parts and 10 ~ 35 mass parts
4~ C
8hydramine and 10 ~ 40 mass parts C
10~ C
18lipid acid helps defoamer with 5 ~ 15 mass parts again at 70 ~ 150 DEG C of esterifications, 30 ~ 150 minutes products therefroms, and 3 ~ 8 mass parts dispersion agents, at the product that 20 ~ 80 DEG C obtain with water mixing and emulsifying for 1 ~ 4 hour.But the defoamer of this invention has antifoaming speed soon, presses down bubble ability strong, particularly has well bubble effect the multiple negatively charged ion commonly used for rubber, plastics-production system, nonionic foaming agent.
The defoamer of above-mentioned prior art mainly due to the COD that can increase waste water after a large amount of use, thus causes secondary pollution.Due to the complicated component of waste water, and with strong acid alkalescence.Therefore need to design that a defoaming capacity is strong and to press down the bubble time long, strong alkali-acid resistance, while can not increase the dedicated defoamer of system COD.
Summary of the invention
The object of the invention is to the preparation method that a kind of use in waste water treatment defoamer is provided for Problems existing in background technology.
The technical scheme realizing the object of the invention employing is: a kind of preparation method of use in waste water treatment defoamer, and its preparation process is as follows:
1) modification of organic silicone oil
Containing hydrogen silicone oil is mixed with polyethers, through Speier catalyst action, obtained polyether modified silicon oil, whole reaction system blanketing with inert gas, system temperature of reaction is 200 ~ 300 DEG C, and the reaction times is 8 ~ 10 hours;
2) preparation of silicon cream
Hydrophabic silica is mixed with dimethyl silicone oil, heated and stirred, make translucent silicon cream;
3) defoamer is composite
Polyether modified silicon oil, step 2 by obtained for step 1)) obtained silicon cream, emulsion adjuvant mix with water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
Wherein, the mass ratio of the containing hydrogen silicone oil described in step 1) and polyethers is 1.2 ~ 1.5, preferably 1:1.3, and the consumption of described Speier catalyzer is 0.4% ~ 0.5% of containing hydrogen silicone oil and polyethers weight sum.
Preferably, in step 1), the molecular weight of described containing hydrogen silicone oil is 5000 ~ 10000.
More preferably, in step 1), described polyethers is ethylene oxide propylene oxide copolyether, and its EO/PO ratio is 0.5 ~ 0.6.
Further preferably, step 2) described in hydrophabic silica and the mass ratio of dimethyl silicone oil be 1:8 ~ 12, preferably 1:8 ~ 10, most preferably 1:9.
Moiety and the percentage composition of defoamer obtained in step 3) are: polyether modified silicon oil 4 ~ 8%, silicon cream 10 ~ 15%, emulsion adjuvant 5 ~ 10%, surplus are water.
Still more preferably, step 2) described in silicon cream preparation also comprise modified manometer silicon dioxide, this modified manometer silicon dioxide is obtained by following steps modification: 1) be dissolved in deionized water by citric acid and form solution, regulator solution pH=4 ~ 5, add nano silicon, high-speed stirring; 2) carry out constant temperature back flow reaction, temperature of reaction is 80 ~ 95 DEG C, and reaction times 0.5 ~ 2h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano silicon of obtained modification.
Wherein, described citric acid and the mass volume ratio of deionized water are 1g:5mL, and described nano silicon and the mass ratio of citric acid are 1:(1 ~ 3).
Technological merit of the present invention is:
1) defoamer that the inventive method is obtained, adopts the organic silicone oil that chemical stability is good, after polyether-modified, forms with silicon cream, emulsion adjuvant etc. are composite.It is strong that this defoamer chemical stability is strong, strong alkali-acid resistance, froth breaking press down bubble ability, and addition is few, but the bubble time is long, and this product can not increase the COD of waste water, avoids the secondary waste water caused owing to the addition of defoamer to pollute.
2) key point of the present invention is the ratio of polyether-modified link and silicone oil used and polyethers, and controls the temperature and time of reaction process.
3) also contain modified manometer silicon dioxide in silicon cream preparation of the present invention, the defoaming capacity of dimethyl silicone oil can be improved, and the froth breaking stability of defoamer.
4) select citric acid to the hydroxyl generation bonding reaction of nano-silica surface, make not easily to reunite between nanometer silicon dioxide particle, improve the dispersing property of nano silicon in froth breaking emulsion.
Embodiment
Below in conjunction with embodiment the present invention done and describe further.
The preparation method of a kind of use in waste water treatment defoamer of the present invention, its preparation process is as follows:
1) modification of organic silicone oil
Containing hydrogen silicone oil is mixed with polyethers, through Speier catalyst action, obtained polyether modified silicon oil, whole reaction system blanketing with inert gas;
2) preparation of silicon cream
Hydrophabic silica is mixed with dimethyl silicone oil, heated and stirred, make translucent silicon cream;
3) defoamer is composite
Polyether modified silicon oil, step 2 by obtained for step 1)) obtained silicon cream, emulsion adjuvant mix with water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
embodiment 1
1) by 50 gram molecular weights be 5000 containing hydrogen silicone oil be that 0.5 polyethers mixes with 60 grams of EO/PO ratios, add 0.4 gram of Speier catalyzer, temperature of reaction is 200 DEG C, reacts 8 hours obtained polyether modified silicon oils, for subsequent use, whole reaction system blanketing with inert gas;
2) 20 grams of hydrophabic silicas are mixed with 160 grams of dimethyl silicone oils, be heated to 50 DEG C of stirrings, make translucent silicon cream;
3) by obtained for 40 grams of step 1) polyether modified silicon oil, 150 grams of steps 2) obtained silicon cream, 50 grams of emulsion adjuvants mix with 760 grams of water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
embodiment 2
1) by 50 gram molecular weights be 6000 containing hydrogen silicone oil be that 0.6 polyethers mixes with 65 grams of EO/PO ratios, add 0.45 gram of Speier catalyzer, temperature of reaction is 250 DEG C, reacts 9 hours obtained polyether modified silicon oils, for subsequent use, whole reaction system blanketing with inert gas;
2) 20 grams of hydrophabic silicas are mixed with 180 grams of dimethyl silicone oils, be heated to 50 DEG C of stirrings, make translucent silicon cream;
3) by obtained for 60 grams of step 1) polyether modified silicon oil, 100 grams of steps 2) obtained silicon cream, 100 grams of emulsion adjuvants mix with 740 grams of water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
embodiment 3
1) by 50 gram molecular weights be 10000 containing hydrogen silicone oil be that 0.54 polyethers mixes with 70 grams of EO/PO ratios, add 0.5 gram of Speier catalyzer, temperature of reaction is 300 DEG C, reacts 10 hours obtained polyether modified silicon oils, for subsequent use, whole reaction system blanketing with inert gas;
2) 20 grams of hydrophabic silicas are mixed with 200 grams of dimethyl silicone oils, be heated to 50 DEG C of stirrings, make translucent silicon cream;
3) by obtained for 80 grams of step 1) polyether modified silicon oil, 120 grams of steps 2) obtained silicon cream, 70 grams of emulsion adjuvants mix with 730 grams of water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
embodiment 4
1) by 50 gram molecular weights be 10000 containing hydrogen silicone oil be that 0.54 polyethers mixes with 75 grams of EO/PO ratios, add 0.5 gram of Speier catalyzer, temperature of reaction is 250 DEG C, reacts 10 hours obtained polyether modified silicon oils, for subsequent use, whole reaction system blanketing with inert gas;
2) 20 grams of hydrophabic silicas are mixed with 240 grams of dimethyl silicone oils, be heated to 50 DEG C of stirrings, make translucent silicon cream;
3) by obtained for 70 grams of step 1) polyether modified silicon oil, 130 grams of steps 2) obtained silicon cream, 60 grams of emulsion adjuvants mix with 740 grams of water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
Embodiment 1 ~ 4 aims at the composite waterborne organic silicon defoamer of wastewater treatment, can rapid dispersion, not easily floating oil in water, and antifoaming speed is fast, presses down bubble lasting, can not increase the COD in waste water, avoid the secondary pollution causing water body, have better resistance to acids and bases.Without physiologically active, corrosion-free, nontoxic, without adverse side effect, do not fire, not quick-fried, safety high.Embodiment 5 be select commercially available defoamer GP330, embodiment 6 selects commercially available defoamer FAG470.The concrete change of COD after using front COD and using, in table 1.
Table 1
Through orthogonal test, the present invention can show that best temperature of reaction is 200 ~ 300 DEG C, reaction times is 8 ~ 10 hours, catalyst levels is 0.4 ~ 0.5%, and the ratio of silicone oil and polyethers is lower, namely content of polyether is higher, reaction conversion ratio is higher, but the simultaneously composite COD of defoamer to water body is higher.By testing selected silicone oil: best during polyethers=1:1.3.
In order to improve the defoaming capacity of dimethyl silicone oil, and the froth breaking stability of defoamer.In the step of embodiment 1 ~ 4 silicon cream preparation, also add modified manometer silicon dioxide.Modified manometer silicon dioxide is obtained by following steps modification: 1) be dissolved in deionized water by citric acid and form solution, regulator solution pH=4 ~ 5, add nano silicon, high-speed stirring; 2) carry out constant temperature back flow reaction, temperature of reaction is 80 ~ 95 DEG C, and reaction times 0.5 ~ 2h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano silicon of obtained modification.Wherein, described citric acid and the mass volume ratio of deionized water are 1g:5mL, and described nano silicon and the mass ratio of citric acid are 1:(1 ~ 3).
It should be noted that, the embodiment described in this specification sheets, its formula, title that technique is named etc. can be different.The equivalence that structure, feature and the principle of every foundation described in inventional idea of the present invention are done or simple change, be included in the protection domain of patent of the present invention.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described embodiment; only otherwise depart from structure of the present invention or surmount the scope that this claim defines, all protection scope of the present invention is belonged to.
Claims (7)
1. a preparation method for use in waste water treatment defoamer, is characterized in that preparation process is as follows:
1) modification of organic silicone oil
Containing hydrogen silicone oil is mixed with polyethers, through Speier catalyst action, obtained polyether modified silicon oil, whole reaction system blanketing with inert gas, system temperature of reaction is 200 ~ 300 DEG C, and the reaction times is 8 ~ 10 hours;
2) preparation of silicon cream
Hydrophabic silica is mixed with dimethyl silicone oil, heated and stirred, make translucent silicon cream;
3) defoamer is composite
Polyether modified silicon oil, step 2 by obtained for step 1)) obtained silicon cream, emulsion adjuvant mix with water, and high-speed stirring, namely obtains use in waste water treatment defoamer.
2. the preparation method of a kind of use in waste water treatment defoamer according to claim 1, it is characterized in that: the mass ratio of the containing hydrogen silicone oil described in step 1) and polyethers is 1:1.2 ~ 1.5, preferably 1:1.3, the consumption of described Speier catalyzer is 0.4% ~ 0.5% of containing hydrogen silicone oil and polyethers weight sum.
3. the preparation method of a kind of use in waste water treatment defoamer according to claim 1, it is characterized in that: in step 1), the molecular weight of described containing hydrogen silicone oil is 5000 ~ 10000, and described polyethers is ethylene oxide propylene oxide copolyether, and its EO/PO ratio is 0.5 ~ 0.6.
4. the preparation method of a kind of use in waste water treatment defoamer according to claim 1, is characterized in that: step 2) described in hydrophabic silica and the mass ratio of dimethyl silicone oil be 1:8 ~ 12, preferably 1:8 ~ 10, most preferably 1:9.
5. the preparation method of a kind of use in waste water treatment defoamer according to claim 1, is characterized in that: moiety and the percentage composition of defoamer obtained in step 3) are: polyether modified silicon oil 4 ~ 8%, silicon cream 10 ~ 15%, emulsion adjuvant 5 ~ 10%, surplus are water.
6. the preparation method of a kind of use in waste water treatment defoamer according to claim 1, it is characterized in that: step 2) described in silicon cream preparation also comprise modified manometer silicon dioxide, this modified manometer silicon dioxide is obtained by following steps modification: 1) be dissolved in deionized water by citric acid and form solution, regulator solution pH=4 ~ 5, add nano silicon, high-speed stirring; 2) carry out constant temperature back flow reaction, temperature of reaction is 80 ~ 95 DEG C, and reaction times 0.5 ~ 2h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano silicon of obtained modification.
7. the preparation method of a kind of use in waste water treatment defoamer according to claim 6, it is characterized in that: described citric acid and the mass volume ratio of deionized water are 1g:5mL, described nano silicon and the mass ratio of citric acid are 1:(1 ~ 3).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107130459A (en) * | 2017-05-19 | 2017-09-05 | 山东佑震化工有限公司 | A kind of black liquid defoamer and its preparation method and application |
| CN108501476A (en) * | 2018-03-14 | 2018-09-07 | 合肥远科服装设计有限公司 | A kind of cold-proof processing technology for taking thermal insulation material |
| CN108970182A (en) * | 2018-07-12 | 2018-12-11 | 杨帮燕 | A kind of stable type defoaming agent and preparation method thereof |
| CN109011726A (en) * | 2018-09-26 | 2018-12-18 | 天津长芦海晶集团有限公司 | Acidproof resistance to high temperature resistant type defoaming agent with high salt of one kind and preparation method thereof |
| CN109248470A (en) * | 2017-07-13 | 2019-01-22 | 广州崃克保化工有限公司 | A kind of environment-friendly type aqueous defoaming agent |
| CN109395435A (en) * | 2018-11-06 | 2019-03-01 | 江苏赛欧信越消泡剂有限公司 | A kind of preparation method of high temperature resistant highly basic silicon cream |
| CN109734971A (en) * | 2019-01-11 | 2019-05-10 | 亓明芳 | A kind of light wear-resistant rubber soles |
| CN112376319A (en) * | 2020-10-29 | 2021-02-19 | 江苏利宏科技发展有限公司 | Defoaming agent for papermaking and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107130459A (en) * | 2017-05-19 | 2017-09-05 | 山东佑震化工有限公司 | A kind of black liquid defoamer and its preparation method and application |
| CN109248470A (en) * | 2017-07-13 | 2019-01-22 | 广州崃克保化工有限公司 | A kind of environment-friendly type aqueous defoaming agent |
| CN108501476A (en) * | 2018-03-14 | 2018-09-07 | 合肥远科服装设计有限公司 | A kind of cold-proof processing technology for taking thermal insulation material |
| CN108970182A (en) * | 2018-07-12 | 2018-12-11 | 杨帮燕 | A kind of stable type defoaming agent and preparation method thereof |
| CN109011726A (en) * | 2018-09-26 | 2018-12-18 | 天津长芦海晶集团有限公司 | Acidproof resistance to high temperature resistant type defoaming agent with high salt of one kind and preparation method thereof |
| CN109395435A (en) * | 2018-11-06 | 2019-03-01 | 江苏赛欧信越消泡剂有限公司 | A kind of preparation method of high temperature resistant highly basic silicon cream |
| CN109734971A (en) * | 2019-01-11 | 2019-05-10 | 亓明芳 | A kind of light wear-resistant rubber soles |
| CN112376319A (en) * | 2020-10-29 | 2021-02-19 | 江苏利宏科技发展有限公司 | Defoaming agent for papermaking and preparation method thereof |
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