CN103550961A - Blocky solid defoaming agent and preparation method - Google Patents
Blocky solid defoaming agent and preparation method Download PDFInfo
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Abstract
The invention discloses a blocky solid defoaming agent and a preparation method. The blocky solid defoaming agent comprises the following components in parts by weight: 10-90 parts of fatty acid salts, 1-20 parts of active ingredients, 0-10 parts of emulsifying agent, 10-90 parts of texturing agent, and a proper amount of acid-base modifier. The preparation method comprises the steps: firstly enabling the fatty acid and a sodium hydroxide solution, which are well mixed according to a proportion, to perform neutralization reaction to produce fatty acid salts, then emulsifying the active ingredients through the emulsifying agent, compounding the active ingredients and the fatty acid salts as well as texturing agent, evenly mixing, then properly adding the acid-base modifier, cooling and discharging and filling a plastic bag, and further cooling and molding to obtain solid block products. The preparation method is simple in production process, simple and convenient to operate, excellent in safety, non-toxic, corrosion-free, good in environment compatibility, and free from environment pollution. The product is low in surface tension, fast to disperse in water, fast to defoam, long in foaming inhibition time, less in usage amount, wide in raw material source, high in cost performance, not only is used for papermaking, sewage treatment industry, but also is applicable to petroleum, beneficiation, chemical engineering and other industries.
Description
Technical field
The invention belongs to chemical technology field, relate to industrial defoaming agent, especially a kind of blocks of solid defoamer and preparation method.
Technical background
Pure liquid can not form stable foam, and sneaked in liquid, has after surface-active material, stirs this liquid, and the air entering in liquid has formed stabilising dispersions in liquid medium, just can form stable foam.Most production process foams can bring difficulty to production, can make product quality be affected, and therefore must restrain and bubble or eliminate foam.
Bubble and foam can be used, such as flotation, washing, fire extinguishing, dedusting, manufacture foamed plastics etc.; Bubble and foam also must be eliminated, production processes such as fermentation, coating, papermaking, boiler feed water, sewage disposal, printing and dyeing, and now, foam brings harm to producing, and overcome foam harm, in numerous industry production, all adopts the method that adds defoamer.
By states of matter, divide the kind of defoamer, have liquid and solid-state two kinds.At present, most of defoamers are emulsion-type liquid defoamer; Solid defoamer profile is divided again powdery, granular and block three kinds.It is unstable that solid defoamer has overcome liquid defoamer, easily layering, and storage period is short, the disadvantage of transportation inconvenience etc.And block defoamer, it is convenient not only to transport, take care of, and because volume is large, service time can be lasting.The quality of blocks of solid defoamer froth breaking power is except outside the Pass having with active component performance, also relevant with its release, the release speed of active component can regulate block defoamer release according to user's foam liquid temperature, foam liquid flow, flowing velocity, impulse force size when producing, thereby reach, disappears, presses down the object that bubble is effective, consumption is few.At present, that solid defoamer active component has is silicone based, polyethers, polyol fatty acid ester, amide-type, the high alcohol of high-carbon etc., and its carrier has carboxymethyl cellulose, calcium carbonate, sodium phosphate trimer, silica, molecular sieve, diatomite, converted starch, salt, sucrose etc.
Domestic solid defoamer appears at the eighties in last century, and the product of exploitation is mainly in succession:
Chinese patent CN 8510543A in 1985, solid dispersing anti-foaming agent.This patent system is produced a kind of with acid amides, hydrophobic silicon liquid hydrocarbon, dispersant, mineral oil, the composite dispersed defoamer of amide-type solid of glycerine ester.
Chinese patent CN 88105244.2 in 1989, the production method of industrial silicone defoaming agent.This patent is undertaken composite by 1: 10～2: 5 weight ratios with polysiloxanes and multiple edible analog assistant, can obtain efficient Powdered defoamer.
1993, chemical industry in Jiangsu Province research institute Zhang Jihong be take dimethicone, dimethicone-silica, polyether-modified hydrophilic organic silicon and organosilicon emulsion-type defoamer compound as froth breaking active component, take sodium carbonate, silica, zeolite, polyvinyl alcohol, polyvinylacetate-acrylic copolymer, high molecular weight polyether etc. is carrier, and starch, carboxymethyl cellulose, sodium metasilicate, fatty alcohol, fatty acid ester that has been aided with bonding, film forming, package action etc. is mixed into the high silicone oil content of powdery defoamer.
Chinese patent CN 98111116.5 in 1998, defoamer for beans.Invention is mainly calcium carbonate, and all the other are the solid defoamer that tristerin, beans squeeze and acid solution is re-dubbed.
Chinese patent CN 97110150.7 in 1998, a kind of compound defoamer and production technology.By 30～80 parts of glycerin monostearates, 20～60 parts of precipitated calcium carbonates, 2～20 parts of rice bran oils and polyether compound, form graininess defoamer.
2000 torch new product development center, Nian， Nanning City Liao Lin virtues are developed solidifying paste solid defoamer.It is made with fatty acid ester material, and applies in wastewater treatment.China's paper industry, the 9th phase of calendar year 2001.
Within 2002, the Shen Yulong of Tangshan Teachers College department of chemistry, Zhang Jiansheng are developed a kind of YS type SOLID ORGANIC silicon defoaming agent, and it makes Powdered defoamer so that silicone oil, gas-phase silica, compound emulsifying agent, froth breaking synergist, excipient are composite; Chemical science and technology market, 11 phases in 2002.
Korea Spro of Jinan 456 Co., Ltd. Yulin in 2005, Zhang Meisong are with the preparation of the composite a kind of pulverulent solids foam-killing agent in paper-making of success such as methyl-silicone oil, hydroxy silicon oil, PPG oleate, white carbon, sorbierite, secondary octanol, 4A zeolite, salt; Papermaking chemical product, the 6th phase in 2005.
Chinese patent CN 200810182220.5 in 2008, the preparation of oxide anion antifoaming agent.Inventing a kind of is antifoam composition with calcined oxide calcium or calcined magnesia, coordinates resin, auxiliary agent, anionic additive, solid matrix etc. and the female powder defoamer for production process of plastic products is added in raw material of formation.
Chinese patent CN 1010584416.4 in 2010, a kind of solid defoamer and preparation method.This invention carrier (glauber salt, tertiary sodium phosphate, converted starch, zeolite, calcium carbonate and diatomite etc.) account for 50 %～90%, silicone grease is that active component accounts for 5%～20%, emulsifying agent (AEO, polyether-modified polysiloxane, oleic acid polyoxyethylene, alkylol APEO or castor oil polyoxyethylene ether etc.) account for 0.5 %～4 %, structural agent (polyacrylic acid, carboxymethyl cellulose, natrium citricum, potassium citrate and polyvinylpyrrolidone etc.) account for 1 %～30 %, deionized water 5 %～15 %, through the granulation of mixing granulation machine, dry, and must granular solids defoamer.
Chinese patent CN 201210566546.4 in 2012, a kind of preparation method of SOLID ORGANIC silicon defoaming agent.This invention proposes at 130～160 ℃, to make silicon cream with methyl-silicone oil, dimethyl siloxane hydrolysate, white carbon and surface modifier (triethanolamine or n-octyl alcohol), then add polyether modified silicon oil and emulsion adjuvant (APES, APEO, aliphatic acid polyethenoxy ether) to make emulsifiable paste, get 10～20 parts of emulsifiable pastes, 75～95 parts of mixing of carrier (sodium carbonate or sodium acid carbonate), obtain solid defoamer.
Chinese patent CN 201210436193.6 in 2013, solid defoamer and preparation technology thereof.It is raw material that this invention proposes take dimethicone, silica, Arlacel-60, Tween-80, polyethylene glycol, paraffin, through mixing, cooling, forming machine moulding, makes pole shape solid defoamer.
Inventor Chinese patent CN 201010614891.1 in 2010, high-temperature resistant solid defoaming agent and preparation method thereof.This invention proposes with organic silicon modified by polyether, glycerin polyether, glyceride isoreactivity composition after compound emulsifying agent emulsification, composite with complex inorganic salt catalyst, is then dried, pulverizes, sieves, and obtains powdery solid defoamer.
At present, China's solid defoamer is with Powdered or graininess is in the majority, although it can be blended in powder and use, but in mobile foam liquid, use still undesirable, disappear and press down the bad control of bubble ability, and develop a kind of both economy, raw material sources are wide, and adapt to and to use in mobile foam liquid, the convenient blocks of solid defoamer of arbitrarily putting into or taking out at foam liquid is very necessary.
Summary of the invention
The object of the invention is to overcome liquid defoamer unstable, easily layering, storage period is short, and in the time of transportation inconvenience etc. disadvantage, the foam liquid inconvenience that also solves powdery, granular solids defoamer flow state regulates the problem of defoamer consumption at any time.
The present invention is achieved in that
A defoamer, is characterized in that: comprise that following parts by weight of component makes: compound fat hydrochlorate 10～90; Active component 1～20; Emulsifying agent 0～10; Structural agent 10～90; Acid-base modifier is appropriate;
The above compound fat hydrochlorate comprises the salt that aliphatic acid that stearic acid, fixed oil, rosin, coconut oil, palmitic acid, palm oil, laurate, castor oil, urushoil, cottonseed oil, Chinese tallow tree oil, lard, Yang Youzhong are two or more and alkali reaction generate.
The above active component comprises modification organic silicon oil, ethylene bis stearic acid amide, paraffin, sorbitol coconut oil acid ester, glyceryl monostearate,, the two or more chemical substances in tributyl phosphate.
The above emulsifying agent comprises more than one chemical substances in diethylene glycol laurate, spans, APES, quaternary cationics in non-ionic surface active agent, cationic surfactant.
The above structural agent comprises molasses, aluminium polychloride, polyaluminium sulfate, aluminum sulfate, calcium chloride, changes the two or more chemical substances in the swollen Run soil of surname.
More than the above acid-base modifier comprises any in inorganic base, inorganic acid, organic acid.
The preparation method of the above blocks of solid defoamer, comprises the following steps:
(1) neutralization reaction: the requirement according to block product to tough hardness, abrasion resistance, solubility, thermal adaptability, to determine that aliphatic acid kind and proportioning drop into reactor, warming while stirring, when temperature reaches 70 ℃～80 ℃, drips 30 % sodium hydroxide solutions and reacts, when temperature reaches 120 ℃～140 ℃, constant temperature 18 min～22 min, carry out incomplete neutralization reaction, substantially complete dehydration, obtain the melt and dissolved compound fat hydrochlorate of degree of neutralization 90 %～98 %, stand-by;
(2) emulsification: be less than under 100 ℃ of temperature conditions, while stirring active component is added in emulsifying kettle, then non-ionic surface active agent, cationic surfactant are slowly added in active component, at 110 ℃～150 ℃, stir 20 ± 2 min, material is fully mixed, stand-by;
(3) composite: under stirring condition, the active component that emulsification is good slowly to be joined in completely reacted melt and dissolved soap solution, after stirring, then structural agent is added, stir, with acid-base modifier, adjust composite material acid-base value as one sees fit;
(4) cooling packing: composite material is cooled to 85 ℃～95 ℃, packs 2 Kg plastic bag packagings into, then, further cooling curing is shaped to blocks of solid product.
Advantage of the present invention and good effect are:
1, the present invention carries out neutralization reaction with multiple aliphatic acid by certain neutralization ratio, obtaining mixing-in fat hydrochlorate is carrier, again the active component that is emulsified into fine particles is adsorbed on it, with structural agent, adjust tough hardness, abrasion resistance, solubility, thermal adaptability, the suspension degree of solid defoamer, thereby reach froth breaking, press down bubble excellent results.
2, production process of the present invention is simple, and production control is easy, and condition is not overcritical; Product Safety is good, difficult combustion, not quick-fried, nontoxic, corrosion-free, good to environment compatibility, free from environmental pollution.
3, this product surface tension force is low, in water, disperses soon, and froth breaking is fast, but the bubble time is long, and consumption is few, and raw material sources are wide, and price is more suitable, and cost performance is high, has good economic benefit, social benefit and ecological benefits.
4, this product, not only for papermaking, sewage treatment industry, is also applicable to the industries such as oil, ore dressing, chemical industry.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
The specific embodiment
Embodiment 1
First in proportion parts by weight fixed oil is 30 parts, 20 parts of rosin, the fatty acid mixed that palm oil is 10 parts drops into be had in chuck stirred autoclave, be warming up to 80 ± 1 ℃, add by neutralization ratio requirement, at the 30 % liquid sodium hydroxide solution of 95 ± 1 %, fatty acid mixed is carried out to incomplete reaction, neutralization reaction temperature is controlled 126 ℃～130 ℃, after constant temperature 20 ± 2 min, prepare the compound fat hydrochlorate of degree of neutralization 95 %, standby.Then at another little emulsifying kettle, add 3 parts of dimethicones, 5 parts, paraffin, 5 parts of glyceryl monostearates, 5 parts of active defoaming agent compositions of ethylene bis stearic acid amide, under 145 ℃～150 ℃ temperature conditions, stir, by 4 parts of emulsifying agent L-80,1 part of mixed surfactant of quaternary ammonium salt cationic emulsifying agent slowly joins in the active component having stirred again, and constant temperature stirs 20 ± 2 min, make active component material fully emulsified, stand-by
.the active component that emulsification is good is joined in completely reacted mixing-in fat hydrochlorate, stir, slowly add 5 parts of structural agent modified alta-muds, 4 parts, aluminum sulfate, 4 parts, calcium chloride, 4 parts, molasses, after continuing to stir, with acid or alkali regulate material acid-base value to pH value 9.The material regulating is cooled to 87 ± 2 ℃, and with the plastic bag packaging material that can fill 2 Kg materials, sealing, horizontal packing material, further cooling curing moulding, obtains rectangular block shape solid defoamer product.
Embodiment 2
First in proportion parts by weight palmitic acid is 30 parts, Chinese tallow tree oil is 20 parts, the fatty acid mixed that rapeseed oil is 10 parts drops into be had in chuck stirred autoclave, be warming up to 70 ± 1 ℃, add by neutralization ratio requirement, at the 30 % liquid sodium hydroxide solution of 90 ± 1 %, fatty acid mixed is carried out to incomplete reaction, neutralization reaction temperature is controlled 120 ℃～125 ℃, after constant temperature 20 ± 2 min, prepare the compound fat hydrochlorate of degree of neutralization 90 %, standby.Then at another little emulsifying kettle, add 8 parts of dimethicones, 3.5 parts of sorbitol coconut oil acid esters, 5 parts of active defoaming agent compositions of glyceryl monostearate, under 120 ℃～125 ℃ temperature conditions, stir, then by 4 parts of emulsifying agent NP-30,0.5 part of mixed surfactant of diethylene glycol Chinese rose acid esters emulsifying agent slowly joins in the active component having stirred, constant temperature stirs 20 ± 2 min, makes active component material fully emulsified, stand-by
.the active component that emulsification is good is joined in completely reacted mixing-in fat hydrochlorate, stir, slowly add 7 parts of structural agent modified alta-muds, 8 parts of superfine alumina silicates, 2 parts of aluminium polychlorides, after 2 parts, molasses continue to stir.With acid or alkali regulate material acid-base value to pH 8.5.The material regulating is cooled to 92 ± 1 ℃, and with the plastic bag packaging material that can fill 2 Kg materials, sealing, horizontal packing material, further cooling curing moulding, obtains rectangular block shape solid defoamer product.
Embodiment 3
First in proportion parts by weight fixed oil is 20 parts, Chinese tallow tree oil is 20 parts, 10 parts of rosin, coconut oil is that the fatty acid mixed input of 10 parts has in chuck stirred autoclave, is warming up to 75 ± 1 ℃, adds by neutralization ratio requirement, at the 30 % liquid sodium hydroxide solution of 96 ± 1 %, fatty acid mixed is carried out to incomplete reaction, neutralization reaction temperature is controlled 130 ℃～135 ℃, after constant temperature 20 ± 2 min, prepare the compound fat hydrochlorate of degree of neutralization 96 %, standby.Then at another little emulsifying kettle, add 10 parts of dimethicones, 3 parts of tributyl phosphates, 5 parts of active defoaming agent compositions of glyceryl monostearate, under 125 ℃～128 ℃ temperature conditions, stir, 2 parts of 3 parts of NP-30 of emulsifying agent S-60 are slowly joined in the active component having stirred, constant temperature stirs 20 ± 2 min, makes active component material fully emulsified again.After emulsification finishes, the active component that compound fat acid and emulsification are good is composite, after stirring, by 4 parts of structural agent modified alta-muds, 6 parts of superfine alumina silicates, 2 parts of polyaluminium sulfates, 3 parts, calcium chloride, 2 parts, molasses slowly add in said mixture under stirring condition, until stir.Regulate material acidity-basicity ph 8.5, control temperature of charge at 86 ± 1 ℃, with the plastic bag packaging material that fills 2 Kg materials, sealing, horizontal packing material, further cooling curing moulding, obtains rectangular block shape solid defoamer product.
Embodiment 4
First in proportion the defoamer carrier components of parts by weight: 20 parts of stearic acid, Chinese tallow tree oil is 20 parts, 10 parts, paraffin, coconut oil is that the fatty acid mixed of 10 parts drops into and to have in chuck stirred autoclave, is warming up to 78 ± 1 ℃, adds by neutralization ratio requirement, at 97 ± 1% 30 % liquid sodium hydroxide solution, fatty acid mixed is carried out to incomplete reaction, neutralization reaction temperature is controlled 120 ℃～125 ℃, after constant temperature 20 ± 2 min, prepare the compound fat hydrochlorate of degree of neutralization 97 %, standby.Then at another little emulsifying kettle, add 10 parts of dimethicones, 3 parts, paraffin, 5 parts of active defoaming agent compositions of glyceryl monostearate, under 115 ℃～125 ℃ temperature conditions, stir, then by 1 part of quaternary ammonium salt cationic emulsifying agent, 4 parts of emulsifying agents of Arlacel-60 slowly join in the active component having stirred, constant temperature stirs 20 ± 2 min, makes active component material fully emulsified.After emulsification finishes, the active component that compound fat acid and emulsification are good is composite, after stirring, by 4.5 parts of structural agent modified alta-muds, 7 parts of superfine alumina silicates, 3.5 parts of polyaluminium sulfates, 2 parts, molasses slowly add in said mixture under stirring condition, until stir.Regulate material acidity-basicity ph 7.5, control temperature of charge 94 ± 1 ℃ of left and right, with the plastic bag packaging material that fills 2 Kg materials, sealing, horizontal packing material, further cooling curing moulding, obtains rectangular block shape solid defoamer product.
The method of testing of blocks of solid defoamer performance:
For defoamer, correct performance test is very important, and this defoamer is tested foam liquid used and adopted paper-making industry foaming medium, simultaneously for presence states, test event is defined as to three contents:
(1) mensuration of defoaming effect:
Blocks of solid defoamer sample is made into 10 % solution; Paper mill black liquor (pH=12) 150 ml are placed in to 500 ml marked flasks, start and stir, 300 ml make to bubble, stop stirring, with syringe, extracting 0.5 ml 10 % defoamer solutions adds in flask, start stopwatch, a foam decline ml number of every 40 s records, by the size of time and foam decrease speed relation judgement froth breaking power.Time is shorter, and foam falls sooner, and froth breaking power is for well.
(2) press down the mensuration of bubble effect: after foam no longer declines in (1) flask, restart after stirring 30 min and record foam lifting height, shorter with the time, foam rises sooner, represents to press down bubble power for poor; As both long in the time, non-foam rises again, presses down bubble effect best.
(3) mensuration of abrasion resistance:
In 500 ml there-necked flasks, add deionized water 400 ml, get same block solid defoamer sample, cut square block defoamer 16 g and knock down in flask, start 1500 r/min and stir, overall process constant temperature is 40 ℃, after 20 min, taking-up defoamer weighs, and weight is heavier, and abrasion resistance is better.Repeat 1 time, error is reasonable operation at 5 %.
Product of the present invention and external sample comparative test result are as follows:
Claims (6)
1. a blocks of solid defoamer, is characterized in that: comprise that following parts by weight of component makes: compound fat hydrochlorate 10～90; Active component 1～20; Emulsifying agent 0～10; Structural agent 10～90; Acid-base modifier is appropriate;
The above compound fat hydrochlorate comprises the salt that aliphatic acid that stearic acid, fixed oil, rosin, coconut oil, palmitic acid, palm oil, laurate, castor oil, urushoil, cottonseed oil, Chinese tallow tree oil, lard, Yang Youzhong are two or more and alkali reaction generate.
2. a kind of blocks of solid defoamer according to claim 1, is characterized in that: described active component comprises the two or more chemical substances in modification organic silicon oil, ethylene bis stearic acid amide, paraffin, sorbitol coconut oil acid ester, glyceryl monostearate ester, tributyl phosphate.
3. a kind of blocks of solid defoamer according to claim 1, is characterized in that: described emulsifying agent comprises more than one chemical substances in diethylene glycol laurate, spans, APES, quaternary cationics in non-ionic surface active agent, cationic surfactant.
4. a kind of blocks of solid defoamer according to claim 1, is characterized in that: described structural agent comprises molasses, aluminium polychloride, polyaluminium sulfate, aluminum sulfate, calcium chloride, changes the two or more chemical substances in the swollen Run soil of surname.
5. a kind of blocks of solid defoamer according to claim 1, is characterized in that: more than described acid-base modifier comprises any in inorganic base, inorganic acid, organic acid.
6. the preparation method of a kind of blocks of solid defoamer according to claim 1, is characterized in that: comprise the following steps:
(1) neutralization reaction: the requirement according to block product to tough hardness, abrasion resistance, solubility, thermal adaptability, to determine that aliphatic acid kind and proportioning drop into reactor, warming while stirring, when temperature reaches 70 ℃～80 ℃, drips 30 % sodium hydroxide solutions and reacts, when temperature reaches 120 ℃～140 ℃, constant temperature 18 min～22 min, carry out incomplete neutralization reaction, substantially complete dehydration, obtain the melt and dissolved compound fat hydrochlorate of degree of neutralization 95 %～98 %, stand-by;
(2) emulsification: being less than under 100 ℃ of temperature conditions, while stirring active component is added in emulsifying kettle, then non-ionic surface active agent, cationic surfactant are slowly added in active component, at 110 ℃～150 ℃, stir 20 min, material is fully mixed, stand-by;
(3) composite: under stirring condition, the active component that emulsification is good slowly to be joined in completely reacted melt and dissolved soap solution, after stirring, then structural agent is added, stir, with acid-base modifier, adjust composite material acid-base value as one sees fit;
(4) cooling packing: composite material is cooled to 85 ℃～95 ℃, packs 2 Kg plastic bag packagings into, then, further cooling curing is shaped to blocks of solid product.
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