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CN105152255B - A kind of preparation method of use in waste water treatment defoamer - Google Patents

A kind of preparation method of use in waste water treatment defoamer Download PDF

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CN105152255B
CN105152255B CN201510607976.XA CN201510607976A CN105152255B CN 105152255 B CN105152255 B CN 105152255B CN 201510607976 A CN201510607976 A CN 201510607976A CN 105152255 B CN105152255 B CN 105152255B
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defoamer
silicon
preparation
waste water
water treatment
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CN105152255A (en
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刘鸣
刘利娟
孙宇亮
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SUZHOU JINGXIE HIGH-NEW ELECTRONIC MATERIAL Co Ltd
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SUZHOU JINGXIE HIGH-NEW ELECTRONIC MATERIAL Co Ltd
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Abstract

The invention discloses a kind of preparation method of use in waste water treatment defoamer, belong to water treatment agent field.The preparation process of defoamer of the present invention is as follows:1)The modification of organic silicone oil;2)The preparation of silicon cream;3)The compounding of defoamer.Defoamer made from the inventive method, using the good organic silicone oil of chemical stability, after polyether-modified, is formed with the compounding such as silicon cream, emulsion adjuvant.The defoamer chemical stability is strong, strong alkali-acid resistance, froth breaking suds ability are strong, and addition is few, and the suds time is long, and the product will not increase the COD of waste water, it is to avoid due to the addition of the secondary waste water pollution that defoamer is caused.

Description

A kind of preparation method of use in waste water treatment defoamer
Technical field
The invention belongs to water treatment agent field, and in particular to a kind of preparation method of use in waste water treatment defoamer.
Background technology
A large amount of foams are easily produced in wastewater treatment process, it is necessary to eliminate in time, general periodically addition defoamer.At present Defoamer is broadly divided into three classes:Mineral oils, organic silicon, polyethers.Common defoamer poor chemical stability, and in waste water Complicated component, causes common defoamer floating oil, and foam time is short.
The research of defoamer in recent years be concentrated mainly on the compounding of organo-silicon compound and surfactant, polyethers with it is organic On the compounding of silicon, the water-soluble or Compositional type defoamer such as oil soluble polyether and the compounding of silicon-containing polyether.For current defoamer, Polyethers and the performance of organic silicon defoamer are the most excellent, the developmental research of modification and new varieties to this two classes defoamer Compare active.
Patent No. ZL200410064717.9 discloses a kind of high temperature defoamer and preparation method thereof, and it is by following component Composition:(1)Defoaming activity material:Including the polymerization of organic poly-silicon gas alkane alkane, hydrophobic silicic aerogels, polyoxyethylene and oxypropylene block Thing;(2)Emulsifying agent, organosilyl surfactant;(3)Decentralized medium water.The preparation method of the high temperature defoamer comprises the following steps: (1)Emulsifying agent is first well mixed with defoaming activity thing;(2)Stirring is sufficiently mixed at 50~80 DEG C, adds water in oil and is turned Phase;(3)By step(2)Mixture after middle phase inversion enters colloid mill circulation, then dilutes and can obtain high temperature defoamer.The high temperature defoamer In high temperature degree(60~90 DEG C), with good antifoaming performance and stability;During high temperature Jet Overflow dye, still The good antifoaming performance of energy holding and stability, do not result in dyeing inequality or the defect of specking.
Patent No. ZL200510034583.0 discloses a kind of preparation method of industrial defoaming agent, and its method is first will Glycerine aggregates into the polyglycerol that the degree of polymerization is 2-10 under catalysts conditions, then by definite quality than adding glycerine fatty acid Ester or aliphatic acid carry out ester exchange.The invention production technology is easy, and raw material is easy to get, and froth breaking, suds effect are good, it is adaptable to papermaking, The techniques such as sugaring, fermentation.
Patent No. ZL200410027790.9 discloses a kind of water-soluble defoamer of Nano/micron grade silicon dioxide synthesis And preparation method thereof, the defoamer by particle diameter be silica of the 5~2000nm without hydrophobic treatment, molecular weight be 800~ Dimethicone, polyoxyethylene of 2000 EVA, molecular weight for 15000~60000(4~10)Octylphenol ether, molecular weight Constituted for 1200~2600 propane diols polyoxyethylene poly-oxygen propylene aether;The preparation method of above-mentioned defoamer, comprises the following steps: Silica is subjected to high-temperature process;By the silica after high-temperature process and dimethicone stirring reaction, then add altogether Aggressiveness, continues to pump the water and ethanol of reaction generation after reacting;Add polyoxyethylene(4~10)Octylphenol ether and propane diols polyoxy Ethene polyethenoxy ether, continues to pump the water and ethanol of reaction generation after reacting, room temperature is down to naturally.The invention defoaming effect Good, performance is stable, is suitably applied in high-efficient cutting grinding coolant.
Patent No. ZL01144354.5 discloses a kind of emulsion type defoaming agent, and the defoamer is by 40~60 mass parts The C of alkymer and 10~35 mass parts4~C8Hydramine and 10~40 mass parts C10~C18Aliphatic acid 70~150 DEG C be esterified 30~ 150 minutes products therefroms help defoamer with 5~15 mass parts again, and 3~8 mass parts dispersants mix breast with water at 20~80 DEG C Product obtained by changing 1~4 hour.The defoamer of the invention has antifoaming speed fast, and suds ability is strong, particularly to for rubber The conventional a variety of anion of glue, plastics-production system, nonionic foaming agent have good foam-inhibiting effect.
The defoamer of above-mentioned prior art after a large amount of uses mainly due to that can increase the COD of waste water, so as to cause secondary dirt Dye.Due to the complicated component of waste water, and with strong acid alkalescence.Therefore need to design a defoaming capacity by force and the suds time be long, Strong alkali-acid resistance, while system COD special defoamer will not be increased.
The content of the invention
It is an object of the invention to provide a kind of use in waste water treatment defoamer for problem present in background technology Preparation method.
Realize technical scheme that the object of the invention uses for:A kind of preparation method of use in waste water treatment defoamer, it is prepared Step is as follows:
1)The modification of organic silicone oil
Containing hydrogen silicone oil is mixed with polyethers, through Speier catalyst actions, polyether modified silicon oil, whole reaction system is made Blanketing with inert gas, system reaction temperature is 200~300 DEG C, and the reaction time is 8~10 hours;
2)The preparation of silicon cream
Hydrophabic silica is mixed with dimethicone, heating stirring, translucent silicon cream is made;
3)The compounding of defoamer
By step 1)Obtained polyether modified silicon oil, step 2)Obtained silicon cream, emulsion adjuvant are mixed with water, high-speed stirring Mix, that is, use in waste water treatment defoamer is made.
Wherein, step 1)Described in containing hydrogen silicone oil and polyethers mass ratio be 1.2~1.5, preferably 1:1.3, institute The consumption for the Speier catalyst stated is the 0. 4%~0.5% of containing hydrogen silicone oil and polyethers weight sum.
Preferably, step 1)In, the molecular weight of described containing hydrogen silicone oil is 5000~10000.
It is highly preferred that step 1)In, described polyethers is ethylene oxide propylene oxide copolyether, and its EO/PO ratio is 0.5~0.6.
It is further preferred that step 2)Described in hydrophabic silica and dimethicone mass ratio be 1:8~12, Preferably 1:8~10, most preferably 1:9.
Step 3)In obtained defoamer constituent and percentage composition be:Polyether modified silicon oil 4~8%, silicon cream 10 ~15%, emulsion adjuvant 5~10%, surplus are water.
It is further preferred that step 2)Described in silicon cream prepare and also include modified manometer silicon dioxide, the modification receives Rice silica is modified by following steps and is made:1)Citric acid is dissolved in deionized water and forms solution, regulation pH value of solution=4~ 5, add nano silicon, high-speed stirred;2)Constant temperature back flow reaction is carried out, reaction temperature is 80~95 DEG C, reaction time 0.5 ~2h, carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and is dried, that is, modified nanometer two is made Silica.
Wherein, described citric acid and the mass volume ratio of deionized water are 1g:5mL, described nano silicon with The mass ratio of citric acid is 1:(1~3).
The technological merit of the present invention is:
1)Defoamer made from the inventive method, using the good organic silicone oil of chemical stability, after polyether-modified, with The compounding such as silicon cream, emulsion adjuvant is formed.The defoamer chemical stability is strong, strong alkali-acid resistance, froth breaking suds ability are strong, addition Few, the suds time is long, and the product will not increase the COD of waste water, it is to avoid due to the addition of the secondary waste water that defoamer is caused Pollution.
2)The key point of the present invention is the ratio of polyether-modified link and silicone oil used and polyethers, and controls to react The temperature and time of journey.
3)The silicon cream of the present invention also contains modified manometer silicon dioxide in preparing, and can improve the froth breaking energy of dimethicone Power, and defoamer froth breaking stability.
4)Occur bonding reaction to the hydroxyl of nano-silica surface from citric acid, make nanometer silicon dioxide particle it Between be difficult reunite, improve dispersive property of the nano silicon in froth breaking emulsion.
Embodiment
The present invention is further described through with reference to embodiment.
A kind of preparation method of use in waste water treatment defoamer of the present invention, its preparation process is as follows:
1)The modification of organic silicone oil
Containing hydrogen silicone oil is mixed with polyethers, through Speier catalyst actions, polyether modified silicon oil, whole reaction system is made Blanketing with inert gas;
2)The preparation of silicon cream
Hydrophabic silica is mixed with dimethicone, heating stirring, translucent silicon cream is made;
3)The compounding of defoamer
By step 1)Obtained polyether modified silicon oil, step 2)Obtained silicon cream, emulsion adjuvant are mixed with water, high-speed stirring Mix, that is, use in waste water treatment defoamer is made.
Embodiment 1
1)The containing hydrogen silicone oil for being 5000 by 50 gram-molecular weights with 60 grams of EO/PO ratios is that 0.5 polyethers is mixed, and adds 0.4 gram Speier catalyst, reaction temperature is 200 DEG C, reacts 8 hours obtained polyether modified silicon oils, and standby, whole reaction system is with lazy Property gas shield;
2)20 grams of hydrophabic silicas are mixed with 160 grams of dimethicones, 50 DEG C of stirrings is heated to, is made translucent Silicon cream;
3)By 40 grams of steps 1)Obtained polyether modified silicon oil, 150 grams of steps 2)Obtained silicon cream, 50 grams of emulsion adjuvants with 760 grams of water mixing, high-speed stirred is made use in waste water treatment defoamer.
Embodiment 2
1)The containing hydrogen silicone oil for being 6000 by 50 gram-molecular weights with 65 grams of EO/PO ratios is that 0.6 polyethers is mixed, and adds 0.45 gram Speier catalyst, reaction temperature is 250 DEG C, reacts 9 hours obtained polyether modified silicon oils, and standby, whole reaction system is with lazy Property gas shield;
2)20 grams of hydrophabic silicas are mixed with 180 grams of dimethicones, 50 DEG C of stirrings is heated to, is made translucent Silicon cream;
3)By 60 grams of steps 1)Obtained polyether modified silicon oil, 100 grams of steps 2)Obtained silicon cream, 100 grams of emulsion adjuvants Mixed with 740 grams of water, high-speed stirred, that is, use in waste water treatment defoamer is made.
Embodiment 3
1)The containing hydrogen silicone oil for being 10000 by 50 gram-molecular weights with 70 grams of EO/PO ratios is that 0.54 polyethers is mixed, and adds 0.5 Gram Speier catalyst, reaction temperature is 300 DEG C, reacts 10 hours obtained polyether modified silicon oils, and standby, whole reaction system is used Inert gas shielding;
2)20 grams of hydrophabic silicas are mixed with 200 grams of dimethicones, 50 DEG C of stirrings is heated to, is made translucent Silicon cream;
3)By 80 grams of steps 1)Obtained polyether modified silicon oil, 120 grams of steps 2)Obtained silicon cream, 70 grams of emulsion adjuvants with 730 grams of water mixing, high-speed stirred is made use in waste water treatment defoamer.
Embodiment 4
1)The containing hydrogen silicone oil for being 10000 by 50 gram-molecular weights with 75 grams of EO/PO ratios is that 0.54 polyethers is mixed, and adds 0.5 Gram Speier catalyst, reaction temperature is 250 DEG C, reacts 10 hours obtained polyether modified silicon oils, and standby, whole reaction system is used Inert gas shielding;
2)20 grams of hydrophabic silicas are mixed with 240 grams of dimethicones, 50 DEG C of stirrings is heated to, is made translucent Silicon cream;
3)By 70 grams of steps 1)Obtained polyether modified silicon oil, 130 grams of steps 2)Obtained silicon cream, 60 grams of emulsion adjuvants with 740 grams of water mixing, high-speed stirred is made use in waste water treatment defoamer.
Embodiment 1~4 aim at wastewater treatment compounding waterborne organic silicon defoamer, in water can rapid dispersion, be difficult Floating oil, antifoaming speed is fast, and suds persistently, will not increase the COD in waste water, it is to avoid the secondary pollution of water body is caused, with more preferable Resistance to acids and bases.Corrosion-free, nontoxic, without adverse side effect, non-ignitable, not quick-fried without physiologically active, safety is high.Embodiment 5 is to select Commercially available defoamer GP330, embodiment 6 are to select commercially available defoamer FAG470.Using preceding COD with using the specific of rear COD Change, is shown in Table 1.
Table 1
The present invention can show that optimal reaction temperature is 200~300 DEG C by orthogonal test, and the reaction time is 8~10 Hour, catalyst amount is 0.4~0.5%, and the ratio of silicone oil and polyethers is lower, i.e. content of polyether is higher, and reaction conversion ratio is got over Height, but the defoamer compounded simultaneously is higher to the COD of water body.Pass through the selected silicone oil of experiment:Polyethers=1:It is optimal when 1.3.
In order to improve the defoaming capacity of dimethicone, and defoamer froth breaking stability.In the silicon cream of embodiment 1~4 In the step of preparation, modified manometer silicon dioxide is additionally added.Modified manometer silicon dioxide is modified by following steps and is made:1)By lemon Lemon acid, which is dissolved in deionized water, forms solution, adjusts pH value of solution=4~5, adds nano silicon, high-speed stirred;2)Carry out permanent Warm back flow reaction, reaction temperature is 80~95 DEG C, and 0.5~2h of reaction time carries out suction filtration after completion of the reaction, washs to pH=7, Then it is put in baking oven and is dried, that is, modified nano silicon is made.Wherein, described citric acid and deionized water Mass volume ratio is 1g:5mL, 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, its formula, technique named title etc. can be different. The equivalent or simple change that every construction, feature and principle according to described in inventional idea of the present invention is done, is included in this hair In the protection domain of bright patent.Those skilled in the art can do various to described embodiment Modification or supplement or substituted using similar mode, structure without departing from the present invention or surmount present claims and defined Scope, belong to protection scope of the present invention.

Claims (5)

1. a kind of preparation method of use in waste water treatment defoamer, it is characterised in that preparation process is as follows:
1)The modification of organic silicone oil
Containing hydrogen silicone oil is mixed with polyethers, through Speier catalyst actions, polyether modified silicon oil is made, whole reaction system is with lazy Property gas shield, system reaction temperature be 200~300 DEG C, the reaction time be 8~10 hours;
2)The preparation of silicon cream
Hydrophabic silica is mixed with dimethicone, heating stirring, translucent silicon cream is made;
3)The compounding of defoamer
By step 1)Obtained polyether modified silicon oil, step 2)Obtained silicon cream, emulsion adjuvant are mixed with water, high-speed stirred, i.e., Use in waste water treatment defoamer is made;
Wherein, step 2)Described in silicon cream prepare also include modified manometer silicon dioxide, the modified manometer silicon dioxide by with Lower step, which is modified, to be made:1)Citric acid is dissolved in deionized water and forms solution, pH value of solution=4~5 are adjusted, nano-silica is added SiClx, high-speed stirred;2)Constant temperature back flow reaction is carried out, reaction temperature is 80~95 DEG C, and 0.5~2h of reaction time, reaction is finished After carry out suction filtration, wash to pH=7, be then put in baking oven and be dried, that is, modified nano silicon is made;
Described citric acid and the mass volume ratio of deionized water are 1g:5mL, described nano silicon and the matter of citric acid Amount is than being 1:(1~3).
2. a kind of preparation method of use in waste water treatment defoamer according to claim 1, it is characterised in that:Step 1)Middle institute The containing hydrogen silicone oil and the mass ratio of polyethers stated are 1:1.2~1.5, the consumption of described Speier catalyst is containing hydrogen silicone oil and poly- The 0.4%~0.5% of ether weight sum.
3. a kind of preparation method of use in waste water treatment defoamer according to claim 1, it is characterised in that:Step 1)In, The molecular weight of described containing hydrogen silicone oil is 5000~10000, and described polyethers is ethylene oxide propylene oxide copolyether, its EO/ PO ratios are 0.5~0.6.
4. a kind of preparation method of use in waste water treatment defoamer according to claim 1, it is characterised in that:Step 2)Middle institute The hydrophabic silica and the mass ratio of dimethicone stated are 1:8~12.
5. a kind of preparation method of use in waste water treatment defoamer according to claim 1, it is characterised in that:Step 3)Middle institute The constituent and percentage composition of obtained defoamer be:Polyether modified silicon oil 4~8%, silicon cream 10~15%, emulsion adjuvant 5~ 10%th, surplus is water.
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CN107130459B (en) * 2017-05-19 2018-12-21 山东佑震化工有限公司 A kind of black liquid defoaming agent 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
CN112376319B (en) * 2020-10-29 2021-06-15 江苏利宏科技发展有限公司 A kind of defoamer for papermaking and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1641097A (en) * 2004-12-10 2005-07-20 曹治平 Moderate temperature prnited and dyed organosilicon anti-bubbling and its preparing method
CN102162204A (en) * 2010-02-23 2011-08-24 殷邗清 Method for producing organic silicon defoaming agent for papermaking

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4682116B2 (en) * 2006-10-18 2011-05-11 株式会社神鋼環境ソリューション Organic wastewater treatment method and organic wastewater treatment equipment

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1641097A (en) * 2004-12-10 2005-07-20 曹治平 Moderate temperature prnited and dyed organosilicon anti-bubbling and its preparing method
CN102162204A (en) * 2010-02-23 2011-08-24 殷邗清 Method for producing organic silicon defoaming agent for papermaking

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"聚醚改性硅油消泡剂消泡机理研究";鲁亚青等;《有机硅材料》;20101231;第24卷(第2期);第80页摘要以及第1.1-1.4节实验部分 *

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