CN115317963A - Organic silicon defoaming agent and preparation method thereof - Google Patents
Organic silicon defoaming agent and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
Abstract
The invention provides an organic silicon defoaming agent and a preparation method thereof, belonging to the technical field of papermaking chemicals and comprising the following components in parts by weight: 30.0 to 35.0 parts of organic siloxane; 2.3 to 4.2 parts of polyether modified silicone oil, wherein n (EO) is n (PO) =1, (4.5 to 5); 1.0 to 2.4 parts of propylene caprylate; 1.5 to 2.5 parts of MQ silicon resin; 2.1-3.0 parts of hydrophobic fumed silica, and the D50 is 5-8nm; 0.25-0.40 part of inorganic filler; 2.1 to 2.9 parts of a composite emulsifier, wherein the composite emulsifier is a mixture of a hydrophilic emulsifier and a lipophilic emulsifier, and the HLB of the composite emulsifier is 9.2 to 10.1; 0.2 to 0.5 portion of thickening agent; 50 to 150 parts of deionized water. The defoaming time of the defoaming agent provided by the invention is within 6.1s, the foam inhibition time is more than 61 minutes, and the centrifugal stability and the thermal stability are good.
Description
Technical Field
The invention belongs to the technical field of papermaking chemicals, and particularly relates to an organic silicon defoaming agent and a preparation method thereof.
Background
The paper making process plays an important role in national economy, but with the development of the paper making industry, serious pollution is accompanied, and particularly, the foaming problem is prominent in the paper pulp production and paper making wastewater treatment processes. The main reason is that in the pulping process, the surface tension of the generated saponifiable matter is less than that of black liquor generated by cooking materials, so that the saponifiable matter exists in the surface layer of the black liquor and forms a film, and forms foam under the action of air mixing, and especially, the lower the concentration of the black liquor, the more the foam is, and a large amount of stable foam is easily generated when harder raw materials and raw materials with high resin content are cooked.
The existing defoaming methods comprise a physical defoaming method and a chemical defoaming method, wherein the chemical defoaming method comprises (1) low-carbon alcohols, which can quickly play a defoaming role in an aqueous solution, but has poor foam inhibition capability; (2) The mixture of mineral oil such as fluid paraffin and the surfactant has low cost but general defoaming effect; (3) The defoaming effect of the organic polar compound defoaming agent is general; (4) The organosilicon defoamer has ideal foam breaking and inhibiting performance and is commonly used in the paper making industry. Commonly used silicone defoaming agents are generally prepared into aqueous emulsion products by emulsifying a compound of simethicone and silicon dioxide by using an emulsifying agent, wherein the simethicone has lower surface energy and can be quickly spread in foaming liquid and immersed in foam to break the foam, and meanwhile, the silicon dioxide also has the capability of penetrating the foam, so that the defoaming capability of the defoaming agent is improved. However, the papermaking black liquor has the characteristics of high viscosity, high temperature, strong alkalinity, fine bubbles and the like, and the defoaming and foam inhibiting effects of the common organic silicon defoaming agent are poor, so that a large amount of defoaming agent is required, and the production cost is increased. In the prior art, for example, CN111701284B provides a defoaming agent which can realize defoaming and foam inhibition in black liquor to a certain extent, but the phenomena of demulsification and oil floating can occur in high-temperature and alkaline environments, so that the activity of the defoaming agent is reduced, the defoaming performance is reduced, and the defoaming agent needs to be added repeatedly, thereby increasing the cost of wastewater treatment.
Disclosure of Invention
In order to solve the problems, the invention provides an organic silicon defoaming agent and a preparation method thereof, and the defoaming agent provided by the invention has the advantages of shortening defoaming time, prolonging foam inhibition time and having excellent centrifugal stability and thermal stability by adding quantitative propylene caprylate, controlling the proportion of polyether EO and PO, and limiting proper inorganic fillers and other components.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
on one hand, the invention provides an organic silicon defoaming agent which comprises the following components in parts by weight:
30.0 to 35.0 parts of organic siloxane; 2.3 to 4.2 parts of polyether modified silicone oil, wherein n (EO) is n (PO) =1, (4.5 to 5); 1.0 to 2.4 parts of propylene caprylate; 1.5 to 2.5 parts of MQ silicon resin; 2.1-3.0 parts of hydrophobic fumed silica, and the D50 is 5-8nm; 0.25-0.40 part of inorganic filler; 2.1 to 2.9 parts of a composite emulsifier, wherein the composite emulsifier is a mixture of a hydrophilic emulsifier and a lipophilic emulsifier, and the HLB of the composite emulsifier is 9.2 to 10.1; 0.2 to 0.5 portion of thickening agent; 50 to 150 parts of deionized water.
Furthermore, the organic siloxane consists of dimethyl silicone oil and hydroxyl silicone oil, and the viscosity of the dimethyl silicone oil at 25 ℃ is 0.6-0.8Pa.s; the viscosity of the hydroxyl silicone oil at 25 ℃ is 0.4-0.6Pa.s, and the weight ratio of the dimethyl silicone oil to the hydroxyl silicone oil is 3.5 to 4.
Further, the complex emulsifier is Tween60 and Span60.
Further, the thickening agent is a mixture of hydroxypropyl methyl cellulose and carboxymethyl cellulose, and the weight ratio of the hydroxypropyl methyl cellulose to the carboxymethyl cellulose is 1.
Further, the M/Q value of the MQ silicon resin is 1-1.5.
Further, the inorganic filler is composed of kaolin and montmorillonite, the content of the kaolin in the kaolin is not less than 90wt%, and the weight ratio of the kaolin to the montmorillonite is 1.2 to 1.5.
On the other hand, the invention provides a preparation method of the organic silicon defoaming agent, which comprises the following steps:
s1, preparing polyether modified silicone oil and weighing the components in parts by weight;
s2, mixing organic siloxane, hydrophobic fumed silica and MQ silicon resin to prepare a silicon paste compound;
s3, mixing the silicon paste compound, polyether modified silicone oil and propylene caprylate to prepare a primary mixture;
and S4, adding an emulsifier, a thickening agent, an inorganic filler and deionized water into the primary mixture to finally obtain the organic silicon defoaming agent.
Further, in the step S1, polyether, hydrogen-containing silicone oil and platinum catalyst are mixed and then react for 1-1.5 hours at the temperature of 100-130 ℃, and then are cooled to 40-50 ℃ to obtain the polyether modified silicone oil.
Further, in the step S3, the silicon paste compound, the polyether modified silicone oil, the propylene caprylate and the platinum catalyst are mixed and then react for 40-60min at 110-120 ℃.
On the other hand, the application of the organosilicon antifoaming agent or the preparation method of the antifoaming agent in papermaking black liquor is provided.
The technical scheme of the invention has the following beneficial effects: according to the invention, by adding propylene caprylate, the molar ratio of polyether EO and PO is improved, when n (EO) =1 (4.5 to 5), the propylene caprylate is 1.0 to 2.4 parts, the inorganic filler comprises montmorillonite and kaolin, the weight ratio of the kaolin to the montmorillonite is 1.2 to 1.5, and the hydroxy silicone oil is added, and the weight ratio of the dimethyl silicone oil to the hydroxy silicone oil is 3.5 to 4, according to tests, the defoaming agent provided by the invention has the defoaming time within 6.1s, the foam inhibition time is more than 61min, the centrifugal stability and the thermal stability are good, and the defoaming agent is superior to other commercial polyether modified silicone defoaming agent commodities.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
The invention provides an organic silicon defoaming agent which comprises the following components in parts by weight: 30.0 to 35.0 parts of organic siloxane; 2.3 to 4.2 parts of polyether modified silicone oil, wherein n (EO) is n (PO) =1, (4.5 to 5); 1.0 to 2.4 parts of propylene caprylate; 1.5 to 2.5 parts of MQ silicon resin; 2.1-3.0 parts of hydrophobic fumed silica, and the D50 is 5-8nm; 0.25-0.40 part of inorganic filler; 2.1 to 2.9 parts of a composite emulsifier, wherein the composite emulsifier is a mixture of a hydrophilic emulsifier and a lipophilic emulsifier, and the HLB of the composite emulsifier is 9.2 to 10.1; 0.2 to 0.5 part of a thickening agent; 50 to 150 parts of deionized water.
Under the combined action of the components, 100ml of black liquor of a paper mill is used as a foaming substance, 0.01g of the defoaming agent provided by the invention is added, the foaming is carried out circularly through a foaming machine, the gas flow is 200ml/min, and the timing is started until the foam reaches 500ml, so that the foam inhibition time is not less than 60min; when the foam reaches 500ml, stopping blowing, and recording the complete foam elimination time as the defoaming time, wherein the defoaming time is not more than 10s; taking 5g of a defoaming agent sample, adding 50g of black liquor, raising the temperature to 80 ℃, and standing for 30 hours without floating oil; 15ml of defoamer sample is taken and centrifuged for 30min under the condition of 3000r/min, and the stability is excellent.
The defoaming agent provided by the invention is preferably prepared in the following way:
s1, preparing polyether modified silicone oil and weighing the components in parts by weight.
The polyether is dehydrated in vacuum, hydrogen-containing silicone oil and platinum catalyst are added under the protection of nitrogen, and the mixture is stirred and reacts for a certain time at a certain temperature to obtain the polyether modified silicone oil. The polyether is selected from polypropylene alcohol polyoxyethylene ether, wherein n (EO) n (PO) =1 (4.5 to 5). The hydrogen-containing silicone oil can be one or more of methyl hydrogen-containing silicone oil, methyl terminal hydrogen-containing silicone oil, ethyl hydrogen-containing silicone oil and methyl ethyl hydrogen-containing silicone oil, the viscosity of the hydrogen-containing silicone oil is preferably 0.2-0.5Pa.s, and the hydrogen content is 0.14-0.16mol%;
n (Si-H) = 1.1 to 1.3; the platinum catalyst is an alcoholic solution of chloroplatinic acid.
S2, mixing organic siloxane, hydrophobic fumed silica and MQ silicon resin to prepare a silicon paste compound;
specifically, the organosilane, the hydrophobic fumed silica, the MQ silicon resin and the platinum catalyst are stirred and uniformly mixed, heated to 100-130 ℃ for reaction for 1-1.5 hours, and then cooled to 40-50 ℃.
The organic siloxane comprises dimethyl silicone oil and hydroxyl silicone oil, wherein in order to achieve a better synergistic cooperation effect and improve the stability and foam inhibition performance of the defoaming agent at high temperature, the viscosity of the dimethyl silicone oil at 25 ℃ is 0.6-0.8Pa.s; the viscosity of the hydroxyl silicone oil at 25 ℃ is 0.4-0.6Pa.s, and the weight ratio of the dimethyl silicone oil to the hydroxyl silicone oil is 3.5 to 4; the hydrophobic fumed silica is selected from Wingnewgsai, technical grade, and the particle size D50 of the silica is 5-8nm; the specific surface area is 200-280m 2 (ii)/g; MQ silicon resin is preferably 8206A produced by Jiangxi Xinjiayi new material Co., ltd, and has the M/Q value of 1-1.5。
S3, mixing the silicon paste compound, polyether modified silicone oil and propylene caprylate to prepare a primary mixture;
specifically, the silicon paste compound, the polyether modified silicone oil, the propylene caprylate and the platinum catalyst are stirred and mixed uniformly, and then the temperature is increased to 110-120 ℃ for reaction for 40-60min.
The propylene octanoate is selected from Shanghai Michelle chemical technology, inc.
And S4, adding an emulsifier, a thickening agent, an inorganic filler and deionized water into the primary mixture to finally obtain the organic silicon defoaming agent.
Specifically, adding a composite emulsifier, a thickener and an inorganic filler into the primary mixture, stirring, heating to 50-70 ℃, adding 50-70 ℃ deionized water, shearing for 1-1.5 hours under the condition of 2500-3000r/min, and cooling to obtain the organic defoaming agent.
Specifically, the emulsifier is a composite emulsifier, a mixture of a hydrophilic emulsifier and a lipophilic emulsifier is adopted, and the HLB of the composite emulsifier is 9.2 to 10.1 through blending, wherein the composite emulsifier is Tween60 and Span60; the thickening agent is a mixture of hydroxypropyl methyl cellulose and carboxymethyl cellulose, and the weight ratio of the hydroxypropyl methyl cellulose to the carboxymethyl cellulose is 1 to 2.5. The inorganic filler comprises kaolin and montmorillonite, wherein the content of kaolinite in the kaolin is not less than 90wt%, and the weight ratio of the kaolin to the montmorillonite is 1.2 to 1.5.
Example 1
The embodiment provides an organosilicon defoamer, which comprises the following components in parts by weight: 24.0 parts of dimethyl silicone oil and 6.0 parts of hydroxyl silicone oil; 2.3 parts of polyether modified silicone oil; 1.0 part of propylene caprylate; 1.5 parts of MQ silicon resin; 2.1 parts of hydrophobic fumed silica; 0.11 part of kaolin; 0.14 part of montmorillonite; 2.1 parts of a composite emulsifier; 0.2 part of thickening agent; 50.0 parts of deionized water.
The preparation method comprises the following steps:
s1, carrying out vacuum dehydration on polyether, adding hydrogen-containing silicone oil and a platinum catalyst under the protection of nitrogen, stirring, and reacting for a certain time at a certain temperature to obtain polyether modified silicone oil. The polyether is selected from the group consisting of polyoxypropylene polyoxyethylene ether, wherein n (EO) = n (PO) = 1.
S2, stirring and uniformly mixing 24.0 parts of dimethyl silicone oil, 6.0 parts of hydroxyl silicone oil, 2.3 parts of polyether modified silicone oil, 1.5 parts of MQ silicone resin and a platinum catalyst, heating to 100 ℃, reacting for 1 hour, and cooling to 40 ℃ to obtain a silicon paste compound.
S3, stirring and mixing the silicon paste compound, 2.3 parts of polyether modified silicone oil, 1.0 part of propylene caprylate and a platinum catalyst uniformly, and then heating to 110 ℃ for reaction for 40min to obtain a primary mixture.
S4, adding 2.1 parts of a composite emulsifier with HLB of 9.2, 0.2 part of a thickening agent, 0.11 part of kaolin and 0.14 part of montmorillonite into the primary mixture, uniformly mixing, stirring and emulsifying at a constant temperature of 50 ℃, adding 50 ℃ deionized water, shearing for 1 hour at a shearing speed of 3000r/min, and cooling to obtain the organic silicon defoaming agent.
Example 2
The embodiment provides an organosilicon defoamer, which comprises the following components in parts by weight: 24.0 parts of dimethyl silicone oil and 6.0 parts of hydroxyl silicone oil; 3.0 parts of polyether modified silicone oil; 1.5 parts of propylene caprylate; 2.0 parts of MQ silicon resin; 2.5 parts of hydrophobic fumed silica; 0.13 part of kaolin; 0.17 part of montmorillonite; 2.3 parts of a composite emulsifier; 0.3 part of thickening agent; 80.0 parts of deionized water.
The preparation method comprises the following steps:
s1, carrying out vacuum dehydration on polyether, adding hydrogen-containing silicone oil and a platinum catalyst under the protection of nitrogen, stirring and reacting for a certain time at a certain temperature to obtain polyether modified silicone oil. The polyether is selected from the group consisting of polyoxypropylene polyoxyethylene ether, wherein n (EO) = n (PO) = 1.
S2, stirring and uniformly mixing 24 parts of dimethyl silicone oil, 6 parts of hydroxyl silicone oil, 3.0 parts of polyether modified silicone oil, 2.0 parts of MQ silicone resin and a platinum catalyst, heating to 110 ℃, reacting for 1.2 hours, and cooling to 50 ℃ to obtain the silicon paste compound.
And S3, uniformly stirring and mixing the silicon paste compound, 3.0 parts of polyether modified silicone oil, 1.5 parts of propylene caprylate and a platinum catalyst, and heating to 120 ℃ for reaction for 50min to obtain a primary mixture.
S4, adding 2.3 parts of a composite emulsifier with HLB of 9.5, 0.3 part of a thickening agent, 0.13 part of kaolin and 0.17 part of montmorillonite into the primary mixture, uniformly mixing, stirring and emulsifying at a constant temperature of 60 ℃, adding 60 ℃ deionized water, shearing for 1.5 hours at a shearing speed of 2500r/min, and cooling to obtain the organic silicon defoaming agent.
Example 3
The embodiment provides an organosilicon defoamer, which comprises the following components in parts by weight: 28.0 parts of dimethyl silicone oil and 7.0 parts of hydroxyl silicone oil; 4.0 parts of polyether modified silicone oil; 2.0 parts of propylene caprylate; 2.3 parts of MQ silicon resin; 2.5 parts of hydrophobic fumed silica; 0.18 part of kaolin; 0.22 part of montmorillonite; 2.7 parts of a composite emulsifier; 0.4 part of thickening agent; 120.0 parts of deionized water.
The preparation method comprises the following steps:
s1, carrying out vacuum dehydration on polyether, adding hydrogen-containing silicone oil and a platinum catalyst under the protection of nitrogen, stirring and reacting for a certain time at a certain temperature to obtain polyether modified silicone oil. The polyether is selected from the group consisting of polyoxypropylene polyoxyethylene ether, wherein n (EO) = n (PO) = 1.
S2, stirring and uniformly mixing 28.0 parts of dimethyl silicone oil, 7.0 parts of hydroxyl silicone oil, 4.0 parts of polyether modified silicone oil, 2.3 parts of MQ silicone resin and a platinum catalyst, heating to 1120 ℃, reacting for 1.5 hours, and then cooling to 50 ℃ to obtain the silicon paste compound.
S3, stirring and mixing the silicon paste compound, 4.0 parts of polyether modified silicone oil, 2.0 parts of propylene caprylate and a platinum catalyst uniformly, and heating to 120 ℃ for reacting for 60min to obtain a primary mixture.
S4, adding 2.7 parts of a composite emulsifier with HLB of 9.7, 0.4 part of a thickening agent, 0.18 part of kaolin and 0.22 part of montmorillonite into the primary mixture, uniformly mixing, stirring and emulsifying at a constant temperature of 70 ℃, adding deionized water at a temperature of 70 ℃, shearing for 1 hour at a shearing speed of 3000r/min, and cooling to obtain the organic silicon defoamer.
Example 4
The embodiment provides an organosilicon defoamer, which comprises the following components in parts by weight: 28.0 parts of dimethyl silicone oil and 7.0 parts of hydroxyl silicone oil; 4.2 parts of polyether modified silicone oil; 2.4 parts of propylene caprylate; 2.5 parts of MQ silicon resin; 3.0 parts of hydrophobic fumed silica; 0.15 part of kaolin; 0.21 part of montmorillonite; 2.9 parts of a composite emulsifier; 0.4 part of thickening agent; 150.0 parts of deionized water.
The preparation method comprises the following steps:
s1, carrying out vacuum dehydration on polyether, adding hydrogen-containing silicone oil and a platinum catalyst under the protection of nitrogen, stirring, and reacting for a certain time at a certain temperature to obtain polyether modified silicone oil. The polyether is selected from the group consisting of polyoxypropylene polyoxyethylene ether, wherein n (EO): n (PO) =1: 5.
S2, stirring and uniformly mixing 28.0 parts of dimethyl silicone oil, 7.0 parts of hydroxyl silicone oil, 4.2 parts of polyether modified silicone oil, 2.5 parts of MQ silicone resin and a platinum catalyst, heating to 130 ℃, reacting for 1.5 hours, and cooling to 50 ℃ to obtain the silicon paste compound.
S3, stirring and mixing the silicon paste compound, 4.2 parts of polyether modified silicone oil, 2.4 parts of propylene caprylate and a platinum catalyst uniformly, and heating to 120 ℃ for reacting for 60min to obtain a primary mixture.
S4, adding 2.9 parts of composite emulsifier with HLB of 10.1, 0.5 part of thickening agent, 0.15 part of kaolin and 0.21 part of montmorillonite into the primary mixture, uniformly mixing, stirring and emulsifying at a constant temperature of 50 ℃, adding 70 ℃ deionized water, shearing for 1 hour at a shearing speed of 3000r/min, and cooling to obtain the organic silicon defoaming agent.
Example 5
The embodiment provides an organosilicon defoamer, which comprises the following components in parts by weight: 26.0 parts of dimethyl silicone oil and 6.0 parts of hydroxyl silicone oil; 3.5 parts of polyether modified silicone oil; 2.2 parts of propylene caprylate; 1.7 parts of MQ silicon resin; 2.7 parts of hydrophobic fumed silica; 0.15 part of kaolin; 0.21 part of montmorillonite; 2.5 parts of a composite emulsifier; 0.5 part of thickening agent; 120.0 parts of deionized water.
The preparation method comprises the following steps:
s1, carrying out vacuum dehydration on polyether, adding hydrogen-containing silicone oil and a platinum catalyst under the protection of nitrogen, stirring, and reacting for a certain time at a certain temperature to obtain polyether modified silicone oil. The polyether is selected from the group consisting of polyoxypropylene polyoxyethylene ether, wherein n (EO) = n (PO) = 1.
S2, stirring 26.0 parts of dimethyl silicone oil, 6.0 parts of hydroxyl silicone oil, 3.5 parts of polyether modified silicone oil, 1.7 parts of MQ silicone resin and a platinum catalyst, uniformly mixing, heating to 120 ℃, reacting for 1 hour, and cooling to 50 ℃ to obtain the silicon paste compound.
And S3, uniformly stirring and mixing the silicon paste compound, 3.5 parts of polyether modified silicone oil, 2.2 parts of propylene caprylate and a platinum catalyst, and heating to 120 ℃ for reaction for 60min to obtain a primary mixture.
S4, adding 2.5 parts of a composite emulsifier with HLB of 9.8, 0.5 part of a thickening agent, 0.15 part of kaolin and 0.21 part of montmorillonite into the primary mixture, uniformly mixing, stirring and emulsifying at a constant temperature of 60 ℃, adding 60 ℃ deionized water, shearing for 1 hour at a shearing speed of 3000r/min, and cooling to obtain the organic silicon defoamer.
Comparative example 1
Unlike example 1, this comparative example provides a silicone antifoaming agent in which n (EO) =1 (PO) = 4 of polyether-modified silicone oil in the components.
Comparative example 2
Unlike example 1, this comparative example provides a silicone antifoaming agent in which n (EO) =1 (PO) = 6 of polyether-modified silicone oil in the components.
Comparative example 3
Unlike example 1, this comparative example provides a silicone defoamer in which propylene octanoate is not included in the composition.
Comparative example 4
Unlike example 1, this comparative example provides a silicone defoaming agent in which the content of propylene octanoate in the component is 0.5 parts.
Comparative example 5
Unlike example 1, this comparative example provides a silicone antifoaming agent in which the content of propylene octanoate in the composition was 3.0 parts.
Comparative example 6
Unlike example 1, this comparative example provides a silicone defoaming agent in which the organosiloxane in the composition is dimethicone and does not contain a hydroxy silicone oil.
Comparative example 7
Unlike example 1, this comparative example provides a silicone defoaming agent in which the weight ratio of dimethyl silicone oil and hydroxy silicone oil in the organosiloxane in the composition is 3.
Comparative example 8
Unlike example 1, this comparative example provides a silicone antifoaming agent in which the weight ratio of dimethyl silicone oil and hydroxyl silicone oil in the organosiloxane in the composition is 4.5.
Comparative example 9
Unlike example 1, this comparative example provides a silicone defoamer that does not contain an inorganic filler.
Comparative example 10
Unlike example 1, this comparative example provides a silicone defoamer with an inorganic filler of montmorillonite.
Comparative example 11
Unlike example 1, this comparative example provides a silicone defoamer with an inorganic filler of kaolin.
Comparative example 12
Unlike example 1, this comparative example provides a silicone antifoaming agent, the inorganic filler consisting of kaolin and montmorillonite, wherein the weight ratio of kaolin to montmorillonite is 1.
Comparative example 13
Unlike example 1, this comparative example provides a silicone antifoaming agent, the inorganic filler consisting of kaolin and montmorillonite, wherein the weight ratio of kaolin to montmorillonite is 1.
Comparative example 14 a commercially available polyether modified silicone defoamer, selected from ZJ-800, guangzhou chemical technology ltd.
And (4) testing the defoaming performance, the foam inhibiting performance and the centrifugal stability of the defoaming agent and whether the floating oil exists or not.
Foam inhibition performance: adopting 100ml of paper mill black liquor as a foaming substance, adding 0.01g of the defoaming agent, circularly foaming by a bubbling machine, wherein the gas is nitrogen, the gas flow is 200ml/min, starting timing until the foam reaches 500ml, and obtaining the time as the foam inhibition time.
Defoaming performance: when the foam reaches 500ml, the air blowing is stopped and the time for complete elimination of the foam is recorded, the time obtained being the defoaming time.
Centrifugal stability: and 15ml of a defoaming agent sample is taken and centrifuged for 30min under the condition of 3000r/min, and the stability of the defoaming agent sample is observed.
And (3) taking 5g of a defoaming agent sample, adding 50g of black liquor, raising the temperature to 80 ℃, standing for 30 hours, and observing whether the oil floating phenomenon exists or not. The results of the performance tests are shown in Table 1
TABLE 1 test results of defoaming agent Performance for inventive and comparative examples
From the above examples 1-5, it can be seen that the defoaming time of the silicone defoaming agent provided by the invention is within 6.1s, the foam inhibition time is greater than 61min, and the centrifugal stability and the thermal stability are good; from the data of example 1 and comparative examples 1 and 2, it can be seen that when n (EO) =1 (4.5 to 5) in the polyether-modified silicone oil, the defoaming time is short and the foam suppressing time is long; from example 1 and comparative examples 3-5, it can be seen that when no propylene caprylate is contained, the defoaming agent can generate oil floating phenomenon in black liquor, and more propylene caprylate and less propylene caprylate can affect the action among the components of the whole system, so that the defoaming time is increased, and the foam inhibition time is reduced; as can be seen from the comparison of the data of example 1 and comparative examples 6 to 8, the simethicone alone produces demixing and floating oil, while the hydroxyl silicone oil is more and less, and although the centrifugal stability and the thermal stability are excellent, the foam inhibition time and the foam elimination time are deteriorated; example 1, comparative examples 9-13 it can be seen that the addition of no inorganic filler or only kaolin or only montmorillonite resulted in de-lamination of the defoamer, but not in the unbleached oil; from comparative examples 12 and 13, it can be seen that when the addition ratio is not appropriate, the defoaming time and the foam suppressing time are deteriorated; as can be seen from comparative example 14, compared with the commercial product, the organic silicon defoaming agent provided by the invention greatly improves the foam inhibition time of the defoaming agent in black liquor, shortens the defoaming time, and has good centrifugal stability and thermal stability.
The above description is only an example of the present application and is not intended to limit the scope of the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. The organic silicon defoaming agent is characterized by comprising the following components in parts by weight:
30.0 to 35.0 parts of organic siloxane; 2.3 to 4.2 parts of polyether modified silicone oil, wherein n (EO) is n (PO) =1, (4.5 to 5); 1.0 to 2.4 parts of propylene caprylate; 1.5 to 2.5 parts of MQ silicon resin; 2.1-3.0 parts of hydrophobic fumed silica, and the D50 is 5-8nm; 0.25-0.40 part of inorganic filler; 2.1 to 2.9 parts of a composite emulsifier, wherein the composite emulsifier is a mixture of a hydrophilic emulsifier and a lipophilic emulsifier, and the HLB of the composite emulsifier is 9.2 to 10.1; 0.2 to 0.5 portion of thickening agent; 50 to 150 parts of deionized water.
2. The silicone antifoam agent of claim 1, wherein said organosiloxane is composed of dimethylsilicone oil and hydroxysiloxane oil, and the viscosity of dimethylsilicone oil at 25 ℃ is 0.6 to 0.8pa.s; the viscosity of the hydroxyl silicone oil at 25 ℃ is 0.4-0.6Pa.s, and the weight ratio of the dimethyl silicone oil to the hydroxyl silicone oil is 3.5-4.
3. The silicone antifoam agent of claim 1, wherein said complex emulsifier is Tween60 and Span60.
4. The silicone defoamer according to claim 1, wherein the thickener is a mixture of hydroxypropyl methylcellulose and carboxymethyl cellulose, and the weight ratio of hydroxypropyl methylcellulose to carboxymethyl cellulose is 1.
5. The silicone defoamer of claim 1, wherein the MQ silicone resin has an M/Q value of 1 to 1.5.
6. The silicone defoamer according to claim 1, wherein the inorganic filler is composed of kaolin and montmorillonite, the kaolin has a kaolinite content of not less than 90wt%, and the weight ratio of kaolin to montmorillonite is 1.2 to 1.5.
7. A method of preparing a silicone antifoam agent as set forth in any of claims 1-6, comprising the steps of:
s1, preparing polyether modified silicone oil and weighing the components in parts by weight;
s2, mixing organic siloxane, hydrophobic fumed silica and MQ silicon resin to prepare a silicon paste compound;
s3, mixing the silicon paste compound, polyether modified silicone oil and propylene caprylate to prepare a primary mixture;
and S4, adding an emulsifier, a thickening agent, an inorganic filler and deionized water into the primary mixture to finally obtain the organic silicon defoaming agent.
8. The preparation method according to claim 7, wherein in the step S1, the polyether, the hydrogen-containing silicone oil and the platinum catalyst are mixed and then react at 100-130 ℃ for 1-1.5 hours, and then are cooled to 40-50 ℃ to obtain the polyether modified silicone oil.
9. The method according to claim 7, wherein in step S3, the silicon paste composite, the polyether modified silicone oil, the propylene octoate and the platinum catalyst are mixed and then reacted at 110 to 120 ℃ for 40 to 60min.
10. Use of a silicone defoamer according to any one of claims 1 to 6 or a method of preparing a silicone defoamer according to any one of claims 7 to 9 in black liquor.
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